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| Better Living Through Chemistry Discussions of any and all sorts of mind-warping chemicals, pills, booze, mind machines, trippy stuff, current street prices, importing pharmaceuticals, smart drugs, nutrients, herbs, and altered states. Please try to keep your conversations "theoretical" in nature, since this is an open conference. |
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#1
 2008-11-15, 00:26
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The Exile 
Regular
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BLTC Home Ec - Food for Thought
Hey Totse, just thought I would give everyone some food for thought.
These aren't new and most people know where to find them; however, I figured I would put them on one page for anyone who was interested. Hopefully people might stop asking for them.
Topics included in this post:
How to make:
Methamphetamine synthesis from Psuedoephedrine
Methamphetamine synthesis from P2NP
Methamphetamine synthesis from Ephedrine (Poor quality wright up)
MDMA synthesis from MDP2P
MDMA synthesis from sassafras oil
GBL synthesis from GABA
GHB synthesis from GBL
* I stupidly tried to insert pictures, will have to post links later.
--------------------------------------------------------
Now to begin:
Methamphetamine synthesis from Psuedoephedrine
Complete Newbie Nano
Notes On Newbie Nano:
This is a look at a reaction that has been proven to work. The success in it is utilized and managed by upping the reactants to a higher HI content due to the severe instability of the nano reactions.
The only thing you have to do is figure out how to get clean pseudoephedrine HCL, Clean Matchbook Red Phosphorous, and Clean Iodine.
The ratio for Swims Successful Nano are as follows
5g Pseudoephedrine HCL
5g Matchbook Red Phosphorous
7g Iodine
3mL Dh2o
This ratio will not be to the liking of Wareami or Geezmeister who think the 1/.8/1.2/.5 and 1/.8/1.2/.8 ratio of pse/mbrp/i2/h2o are the way to go.
In a bigger reaction id have to agree, those ratios are very successful. However in Nano conditions there has got to be an excess of HI to compete with such ghetto conditions.
Please remember to always use safety as youre main concern and take every precaution you can think of! Goggles and gloves are very stressed here.
Items For Reaction:
--Precursors--
-Acetone
-Glass coke bottle or Small Glass beer bottle
-Vinyl hose 1' Long
(That fits air tight inside the glass bottle)
-Distilled Water
-Hotplate (using a coil plate would crack the glass!) with thermostat if possible
-Funnel
-Electrical Tape or Duct (duct tape has poor wet adhesion in case of leaks, compared to electrical tape)
-Sandbath
-Small Fan
Making A (Ghetto) Condenser.
Take the 1' Vinyl Hose and fit the punch ballon over one of the ends and tape it on there so its air-tight.
This is your condenser, Set aside.
REACTION
Note: Use a sand bath to heat your glass bottle.
Note: Clean your glass bottle out with water, then acetone and let dry.
Take your glass coke or small beer bottle, place a funnel on top so that when you add the precursors, they will go to the bottom and not get on the walls.
1st: Mix youre pseudoephedrine and Red phosphorous together and then add them to the Flask (glass bottle).
2nd: Add water to the Flask and swirl around gently getting the reactants in contact with the water.
3rd: Get your duct tape and condenser close.
4th: Crush youre iodine and add it to the Flask, quickly add the condenser to the flask and take it on so its air-tight.
Set-your reaction vessel (flask with condenser and balloon), on top of the hot plate but do NOT turn the hot plate on.
The reaction contents should start to liquify and get darker and bubble. Let it do its thing, what you are going to do now is create a very effective Condensing Vessel. After placing the Reaction Vessel on top of the hot plate, put the hot plate near a wall, but do not let it touch the wall, give it an inch between the 2. Then take a piece of duct tape and tape the balloon to the wall so that you have a completely vertical condenser, this will help turn HI(gas) into HI(aq) and will help more than you think! Do not skip this step!
Place a fan facing the condenser and turn it on.
After 20 or so minutes the reaction contents will slow down in bubbling. When this happens turn the hotplate to WARM, this is about 100C. The reaction will gain in size to 3x its original volume, it will react at this volume for an hour or so. When it returns to original volume and slows in reacting, let it sit for another 10 hours. Then turn the heat up to LOW, this will make the volume rise once again, and after an hour or so it will return to normal volume. Let it react on LOW for another 8 hours.
At the end of the reaction, turn off the heat and let the vessel cool to room temp, if your balloon is not flat at the end of the cook, then it should be after the flask cools to room temperature. When the balloon is not inflated anymore, untape it and throw the hose/balloon away.
Post REaction YAY!
Note: Dry All solvents with baked epsom salts before starting the reaction !
Post reaction Items Needed
-Funnel
-2 Glass jars that can hold the funnel and collect liquid
-Distilled Water
-1 Pyrex measuring cup, 500ml of 1000ml
-Hotplate
-Xylene
-VM&P Naptha
-Acetone
-Coffee Filters
-Syphon device (Baby dropper, or eye dropper)
-1 Cotton Ball that fits the neck of the funnel
-25% Naoh Solution (25g of Lye in 100mL of dh2o)
(Note: Make this ahead of time, let it completely dissolve and put in freezer for 30-40 minutes before using)
Take youre reaction vessel and add 75mL of dh2o. Put this on the hotplate and bring it up to a boil, let it boil for 10 minutes (to get rid of excess iodine).
Set-up youre filtering device.
To do this, take the 2 glass jars, put your funnel in one of them, in the funnel neck place a cotton ball firmly in it, on top of this add 1 coffee filter. This works so well because the coffee filter catches all the big solids and the cotton ball collects the small shit that gets through. Pour enough dh2o through the filter to completely wet the filter and cotton ball. discard the water from the jar so that its empty.
Take your reaction vessel after its boiled for 10 minutes, pour it through the wet filter/cotton ball. Add a little more water to the reaction vessel and swirl it around to get the last of the red phosphorous and pour it through the same filter.
Now take the funnel with red phosphorous in it, after all the water has filtered into the 1st jar. Place the funnel in the 2nd jar and take the 1st jar and pour it through the same filter, it will collect in jar 2. Go back and forth 2 times each, a total of 4 times. Then squeeze excess water off of the coffee filter with rp in it. set this aside for future use.
Now you have A glass of what SHOULD be about 100ml crystal clear water. This contains youre methamphetamine, and if you followed directions, very little other shit.
Pour this from the glass jar into the pyrex measuring cup. Add equal amounts of xylene, stir and let it settle. This is a wash of the reaction fluid. Syphon off the xylene (top layer) and discard it.
Now to your washed post reaction fluid, add 200ml of VM&P naptha, put this on the hot plate and put on LOW, this will take 30 minutes to get the naptha hot enough to pull METH, so be patient.
Over the cource of 30 minutes, add a few mL's at a time of youre NaOH Solution. Add a little bit every 5-7 minutes until the bottom is completely milky white, but dont overdue it. The slower you add, the better the migration of freebase meth will be.
Note: Dont listen to anyone that says, dump lye in till you get lye lock, lye in fact does lock the goods up, the molecules need time to migrate.
You can tell if you have overbased because the bottom layer will stay white forever and never become clear again, keep it on the heat till the bottom layer starts to clear from the bottom up. After you the naptha is hot when you touch it, give it another 15 minutes with a little stirring.
Syphon off the Top layer and place it in a glass jar. Do at least two pulls of the rxn fluid with your np. (Standard practice is to do 3 extractions.). Discard the bottom layer, keep the NAptha.
Freezing Naptha
Cover this jar of naptha with a lid or something, place in the freezer for an hour, after you return you should see a crystal clear naptha. If there was any pseudo that hadnt reacted it would show up here. If its crystal clear congrats, go on to the next step
GASSING
Items needed for gassing:
-A large clear plastic jug
-Polyethylene Tubing 1/2' diameter, get 2 feet of this
-Carton of Calcium Chloride
-Muriatic Acid
This is a smelly and violent process so SWIM should do it outside if possible.
Take your bottle, empty it out and clean it out with water, dry it well! After its allowed to dry, fill it half way with calcium chloride.
Take the lid of the jug and make a hold that fits the polyethylene tubing very tightly with no leaks.
When you have this ready, get the muriatic acid and pour about 50-75 ml into the bottle and place the lid on tightly and quickly.
Let this sit for a few minutes, then shake it up a few times and gas will start coming from the end of the tubing, place this in the naptha for 20 or 30 seconds, shake once in a while. The methamphetamine freebase will bond with a HCL molecule.
The now bonded Methamphetamine Hydrochloride will precipitate out as a white salt. It may just look like a cloudy solution at first, let it settle and you will notice that it is salt settling. Get rid of the Gassing jug by safe means, there are many ways to do it safely, just read up and practice before doing this.
Now you have methamphetamine HCL that isnt soluble in naptha. Setup a funnel with 1 coffee filter in it, pour the meth/naptha into the filter and let the naptha drain off. Wash with a little fresh naptha, then while in the same filter, pour some Methyl Ethyl Ketone onto the meth to wash off the naptha and to help dry the meth faster.
Wrap in some coffee filters and then chop up and let dry.
DONE, FINALLY!
You now should have clean methamphetamine ready for consumption.
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#2
 2008-11-15, 00:27
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
Methamphetamine synthesis from P2NP
Making Phenyl-2-Nitropropene
Chemicals
80 mL Toluene (ACS)
40 mL Benzaldehyde (~99%)
30 mL Nitroethane (>99%)
10 mL n-Butylamine (p.a.)
Procedure
The reactants and amine catalysts were dissolved in the toluene in a 250mL RB flask,
boiling stones were added and a Dean-Stark setup was rigged (10mL trap).
The goal was to boil the solution quite heavily to achieve fast dripping from the double surface condenser,
a heating mantle was used.
When the solution had boiled for an hour 2.7mL water was in the trap.
At six hours something like 7.0mL (100% of theory) had settled in the trap.
The solution was dumped into a 250mL beaker, and allowed to cool to room temperature,
it was seeded with some Phenyl-2-Nitropropene crystals, and slowly cooled to around -10°C (freezer).
The crystals looked really nice and no further purification was needed (Yield 35g).
The filtrate was concentrated under vacuum and cooled like above.
Dirty crystals fell and they were recrystallized from 50mL MeOH (Yield 6g).
The total yield from both crops amounted to 41g (64%)
Reducing Phenyl-2-Nitropropene to Phenyl-2-Propane
Chemicals
40,75g Phenyl-2-Nitropropene
115g SnCl2·2H2O
150ml EtOAc
140ml conc HCl
500ml D-H2O
Procedure
Dissolve the tin(II)chloride in water mixed with the hydrochloric acid.
Add the substrate to a RB flask and rinse it all down with the toluene.
Now add the aqueous solution to the RB flask in one portion.
With good stirring bring the mixture to a gentle reflux for 2 hours.
Chill the flask to room temp and saturate the aqueous phase with NaCl, separate the two layers and transfer the top organic layer to a 1L flask containing 500ml water.
Steam distill until no more oily drops comes over.
This means between 500ml to 1.5L distillate is to be collected depending on the volatility of the ketone.
When the steam distillation is over the distillate consits of two layers, one top layer of touene and the major part of the ketone.
Separate the layers in a separatory funnel and extract the aqueous phase with 2x100ml toluene.
Combine the toluene extracts, dry them with MgSO4 and remove the toluene in a rotovap.
Aminating Phenyl-2-Propane to Methyl-Phenyl-Propane-2-Amine
Chemicals
19,75g Phenyl-2-Propane
29.5g Methylamine hcl
19g Aluminiumfoil
500 mg HgCl2
250 ml Isopropanole
100 ml Methanol
450 ml DCM
2730 ml D-H2)
200 ml 25% NaOH solution
200 ml Diethylether
Procedure
In a 1000ml wide-mouthed Erlenmeyer flask, 19 grams of aluminum foil cut to 3x3cm pieces was amalgamated in a solution of 500mg mercuric chloride (HgCl2) in 700ml warm water until the solution became greyish, and hydrogen bubbles was evolved in a steady rate from the aluminum surface.
The water was decanted off, and the aluminum amalgam was washed with 2x500ml cold water.
To the aluminum amalgam there was added 29.5g methylamine hydrochloride dissolved in 30ml hot water, 75 ml isopropanol, 70ml 25% aqueous NaOH,19.75g Phenyl-2-Propanone and finally 175ml isopropanol. Hydrogen was vigorously evolved from the aluminum amalgam, and the temperature of the solution rose quickly.
The reaction rate was controlled by immersing the reaction flask in cold water during 2h, whereafter it was allowed to stand at room temperature with magnetic stirring overnight, with attention being given to the reaction mixture during the first hour so that the temperature did not rise over 50°C.
To the reaction mixture there was added another 50ml 25% NaOH, and the reaction mixture was stirred for 30min and then allowed to settle.
The clear supernatant was decanted, and 100ml isopropanol was added to the grey sludge, and it was stirred for 15min, and the supernatant again decanted.
The aluminum sludge at the bottom of the flask was now filtered through celite in a buchner funnel and washed with 2x50ml Methanol.
All the decantations and washes were combined, and the solution concentrated under vacuum.
The residue was taken up in 1000ml water, acidified by the addition of conc HCl, and washed with 3x50ml DCM, basified with 25% NaOH, and extracted with 3x100ml DCM.
The combined DCM extracts were dried over MgSO4, filtered and the solvent distilled off.
The residue was distilled twice under aspirator vacuum at 100-110°C to give 14.65g (67%) of methamfetamine freebase as a water-white oil.
The hydrochloride salt can be prepared by dissolving the oil in 10x the volume of diethyl ether and gassing the solution with dry HCl gas until no more precipitate forms.
The methamfetamine hydrochloride is filtered off with suction and washed with diethyl ether and air dried.
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#3
 2008-11-15, 00:28
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
Methamphetamine from ephedrine
[QUOTE]
Ok, swim is posting this for info purpose only.
If you follow this exactly it will work for you but for the newbee you need to follow with no subs. This is a long post but f**k it,it will do the job trust swim. Now remember that this can give you many many years in the pen. So anyway,
PART 1A: Acquiring Red Phosphorous
below is SWIM`s own writeup, the long version. totally complete for the new chef and in laymans terms. safety tips included, simple do`s and don't`s that may save the learning chef from harms way. hate to have anyone wind up looking like a match thats already been struck. to the old masters of the game the write up may seem a bit long winded and silly at times but this write up is NOT for you as SWIM is sure you have mastered the RP from MB technique.
heres what SWIM`s insane friend in the big city does.
take your 1000 (1 case) matchbooks and remove the matches by opening the book and ripping out the matches. that will leave you with just the complete cover in your hand. you will get fast and efficient at this with practice. be CAREFUL during this stage, you don't want several hundred ripped out matches catching fire. don't have more than one book in your hand at a time. SWIM`s friend grabs ONE book flips it open holds it in left hand rips matches out with his right hand, throws em in container next to him. the container SWIM uses is a heavy gauge plastic with a tight fitting lid so if you do have a fire in the container the lid can be slammed on thereby smothering the fire. he has seen people rip out matches drop em in there lap etc. and have 4 or 5 empty covers in left hand (which still contains the striker remember) and then next thing you know a book being ripped out accidently catches one of the strikers in left hand and WOOSH. if they are stacked in your lap you can imagine how bad it can be. so one at a time only and don't stack em in your lap. DO NOT open more than one box of 50 at a time for the same reasons. when you are done you will have 1000 strike covers stacked on there sides (minus the matches) in the little cardboard boxes the match books originally came in. 1000 usually fits in 2 of the boxes. next take your good sharp med. size scissors. (fiskars seem to be best in quality) now take ONE at a time and cut the short side off. SWIM`s friend grabs one cover in left hand holding in a way that theres 2 inches or so of cover then the strike pad then a short inch or so of cover (the end where the staple was holding in matches) towards his right hand. cut off the short end right exactly on the line you don't want none of the paint/ink from the cover design with your strike pad. next cut it above the strike pad again exactly on the line. when you cut the strike pad off let it fall into a container by itself (SWIM`s friend uses one of the cardboard boxes that originally held 50 books) sure when you cut them you can cut 3 or 4 at a time but SWIM will take the time to explain why you shouldn't. if you cut more than one at a time the others will move slightly underneath the top one and you will end up with part of the RP cut off on the bottom and part of the paint/ink left on the top of the pads the more you try and cut at once the more pronounced this effect will become towards the last one in the stack. try a few and you will see, or better yet do it as SWIM is telling you since he took the time to type all this shit out in about as layman terms as he can lay it. like he said above, with practice you will become very fast at this. SWIM`s friend and SWIM can do 10 cases (10,000) books in about 4 hours 15 min.. now at this point you should have 1000 strike pads in front of you. SWIM`s friend in the big city now takes them and dumps them in a colander (one of those things you drain spaghetti in) bounce them around in there letting all the little pieces of paper cuttings and the little cardboard pellet looking things from where the staple went thru to hold the matches in originally. you will see when they quit falling out of colander. now its time for the removal of the RP from the strike pads:
PART 1B:
if you are only doing a 1000 books take a quart jar the kind that the mouth is the same diameter as the jar. (skippys peanut butter jars work great)...(the necked down mouths work but its a little harder to get your strike pads out when they are done being soaked) put the pads in the jar, fill with hot water to about 3 inches above the pads. put the lid on, shake the hell out of them. immedieatly pour off the hot water, dont let them soak in the hot water more than 2 minutes or to much paper pulp is introduced. pour off the hot water and discard. now pour acetone or denatuered alcohol on them and shake the hell out of them. let them sit 20 minutes or so and shake them again. all the RP should now be off the pads and you can remove the strike pads. SWIM`s friend uses stainless steel serving tongs to grab a small heap of pads swish them gently around in tone (making sure no clumps of RP are stuck in them) then remove them. repeat this untill all the strike pads you can see are removed. add a little bit more fresh tone and shake the shit up good let it set for a short. now you should have before you a one quart jar with a 1/4 inch or so of reddish/brownish goop/powder on the bottom and 2 to 4 inches of medium to dark maroon tone. you will notice that no matter how long it sets the tone will not lighten up and still look as if it has some RP suspended in it. if it does its miniscule and not worth f**kin with. siphon the tone off into waste can. after that take the RP and put it in a jar and pour in muriatic acid to a couple inches above the RP. bring it to a boil (outside of course) for 5 min or so and then rinse it with DH2O untill you've ran at least a quart thru it. you shouldn't be able to smell ANY muriatic only the unmistakable smell of RP. dry it TOTALLY and its ready to rock. another way that works is take the RP and put it in a 250 to 500 ml boiling flask. (or whatever is large enough to hold the amount you have and hold up to the LOW heat) for every 10 grams of RP put in 1/8 to 1/4 teaspoon of RD lye. add DH2O untill the RP is covered by a 2 or 3 inchs. put it on the hotplate (outside of course) and cook it for 2 hours on LOW LOW heat DO NOT let it boil and DO NOT let the water cook out as the lye will want to erupt if it gets to hot or runs low on water. the lye will cook out of the mix and the caustic nature of it will burn everything out of the RP that isnt RP. keep a close eye on the shit and add more DH2O as needed to keep the RP covered. DO NOT leave it unattended as it will try to climb out of the flask and the flask will need to be removed from the heat and swirled for a few seconds untill it subsides then returned to heat. wash it WELL with DH2O afterwards. run the RP thru a fine sieve strainer to powder it SWIM always does this when it has a miniscule amount of moisture left in it as waiting till its totally bone dry makes the little chunks fly everywhere when you try and run them thru the sieve. after its ran thru the fine sieve dry it the last little bit to bone dry, weigh it and store it in an airtight container. write the weight of the RP on the container you store it in then you dont have to remember.
SWIM`s friend usually yeilds 7 to 10 grams (per 1000 books) of super clean RP this way. as its drying you should grab the bowl every once in awhile and gently mash up the large lumps as they are easier to mash up when its damp than when its bone dry. when hes done its all usually the size of pinheads and smaller and ready for the fine sieve mentioned above. this may seem like a long difficult way to do it but trust me its not. the more you do it the faster you will get. typing all this seems more of a pain in the ass to SWIM than doin the matches... if you are gonna do more than a 1000 books do it in more jars or get a gallon jar, no big deal.
there ya go. simple as it gets. as you do it more and more you will naturally devolop your own little twists and methods and polish and refine your technique. well, some people will but most WILL fail miserably at it and fail at the other steps as well. if everyone could do it then it would be everywhere and wouldnt be worth 2 bucks a gram. if you find yourself to be one of those guys that just cant get it right don`t despair. find a true friend that you trust and teach them the methods you find here and at rhodium and the hive and sponsor them if they have what it takes. SWIM was lucky and took to it like a duck to water. ALWAYS work safe and THINK as you work. it dont take much of a temporary lapse of your power station to bring on disaster and possibly cost you your life and/or liberty.
ACETONE IS A VERY DANGEROUS/FLAMMABLE CHEMICAL AND WILL FLASH TO FIRE WITH LITTLE PROVACATION AND NO WARNING.
DO NOT HEAT IT IN THE MICROWAVE.
DO NOT SMOKE AROUND IT.
EXTINGUISH ALL PILOT LIGHTS ON GAS APPLIANCES (stove top, oven & hot water heater) BE AWARE OF THE FURNACE/HEATING SYSTEM, MOST FORCED AIR UNITS HAVE NO PILOT BUT DO HAVE AN ELECTRONIC IGNITION. TURN IT OFF. YOU MAY HAVE BASBOARD HEAT AND THINK ITS ALL GOOD HOWEVER SOMEWHERE THERES A BOILER THAT HEATS THE LIQUID BEING PUSHED THRU THE BASEBOARD. ITS USUALLY IN THE BASEMENT OR LOWEST PART OF THE HOUSE, THE SAME PLACE THAT THE ACETONE/SOLVENT FUMES WILL MIGRATE TO. IF YOUR NOT SURE WHAT TYPE OF HEAT YOU HAVE OR WHERE THESE APPLIANCES ARE LOCATED MAYBE YOU SHOULD NOT BE ATTEMPTING THIS.
MAKE SURE THERE IS ADEQUATE VENTILATION AND REMEMBER, THE FUMES WILL HUG THE FLOOR AND CAN IGNITE FROM SCOURCES FAR FROM YOUR WORK AREA.
READ THE WARNINGS ON THE CAN AND FOLLOW THEM. THEY MAY SAVE YOUR LIFE, YOUR HOME, YOUR FAMILY, THEY DONT PRINT THE SHIT ON THE CAN CUZ IT LOOKS COOL. THIS SHIT IS NOT CHILDS PLAY.
FOR YOUR OWN SAFETY HEED SWIM`s WORDS
Edit: Be aware of the date of this post as it is old and the pill extraction method below is waaaayyyyy outdated so swim would skip this part and find and updated method on how to aquire your PSE out of all of those gakks.....2/4/06
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#4
 2008-11-15, 00:29
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
Continued:
************************************************** **********************************
PART 2A: Extracting Psuedoephedrine from cold/sinus pills
Chems Needed:
TCE= available at your local auto parts store as BRAKLEEN or ELECTRAMOTIVE made by the CRC company. ingrediants are:
Tetrachloroethylene CAS# 127-18-4 & carbon dioxide CAS# 124-38-9
the tetra is the chemical the carbon dioxide is the propellent. if you are looking at the right can (red & black with a black cap) then these will be the ingrediants. NO SUBSTITUTIONS
Japan Dryer is used when applying varnish or shellac in humid weather. it is added to the varnish or shellac to speed up the drying process. available at hardware stores in the paint section. ingrediants are: Napathenic Salts, Petroleum Distillates.NO SUBSTITUTIONS
the mix desired is 10 to 1
100 ml TCE 10 ml JD per 100 count of 60 mg pills. spray into a clean empty jar the needed amount of TCE. pour in the premeasured amount of JD. shake well and then pour it on the pill mass in the other jar. let it soak with stirring for 3 minutes NO MORE THAN 3 MINUTES. got it? good.
here is the step by step SWIM did in his test run complete with list of active ingrediants and inactives.
ACTIVE INGREDIANTS:
Psudoephedrine HCL .60 mg
tripolidine 2.5 mg
INACTIVE INGREDIANTS:
methylcellulose
lactose
magnesium stearate
polyethylene glycol
silica gel
starch
stearic acid
titanium dioxide
1...ground up 96 (4 boxes of 24 ct) pills with mortar and pestle to a fine powder.
2...passed thru a fine sieve used in canning jellies (its all plastic and works great)
3...measured out 100 ml TCE and 10 ml japan drier. mixed together well and poured onto pill powder in 1 pint jar. stirred well and let set THREE minutes.
4...poured entire jar contents thru a funnel with a single filter and no plug. pill mass was an ugly sorta pale blue/grey. sprayed sides of filter down with TCE from the spray can with tube attached. when all pill mass was in bottom of filter it was removed twisted and rung out.
5...opened filter and spread pill mass out on glass plate. as it dried the small clumps were chopped smaller with razor blade. it was left to set untill it was totally bone dry.
6...the dried pill mass was passed thru the fine sieve again. (a side note of caution here, to avoid the wrath of the wife buy your own fine sieve strainer from canning section of store. dont use hers as it will smell of japan drier untill the end of the time)
7...placed pill mass in clean pint jar. poured in 250 ml of denatured alcohol. stirred let set untill clear. decanted, evapped,
repeated two more times.
8...took the bone dry scrapings from 3 evaps (they were ugly blue/grey (but SWIM had faith and was not worried) ran them through the fine sieve strainer again, poured 100 ml of COLD DRY acetone on the crystals and stirred and stirred and voila white crystals crashing out of tone and the tone was now the ugly blue/grey color. decanted tone, spread crystals out on plate to finish drying and they were beautiful snow white crystals. SWIM had to put on his sunglasses they were so white. they were again passed thru the fine sieve strainer, weighed and stored in an airtight, light proof container. ready to join the other two reagents in the flask when the time comes.
IMPORTANT NOTES:
1. this extraction method was formulated for white 60`s. reports have come in that say it works across the board on a multitude of pills including redhots (deredded 1st of course) and 120`s. these reports are from very reliable scources however SWIM has only done it personally on white 60`s which it was designed around and for. if you dont know what white 60`s , redhots and 120`s are then you are no where near ready to do this and need to research further in labtips. do your research 1st by reading thru all the past pages in labtips. read ALL the threads. the information there is invaluable. then when you have questions about your research post your questions in a thread. the folks there will gladly help. however be warned that questions asked without research 1st such as: "hey man i need a quick easy recipie to make meth" or: "ive searched and searched and cant find -fill in the blank-". posts such as these will be promptly ignored or will result in you being flamed to a crisp, most likely the latter. and believe SWIM the folks there will know if you have done your homework and are in need of help or if you are simply trying to go the easy lazyass way. they are not easily fooled as they have been doing this for a long time. some of them longer than some of you have been alive.
2. it is very important that at the beginning and between each step where noted the pill mass be passed thru the fine sieve strainer. chopping with a razor blade or crushing with mortar and pestle simply wont get it. the mass needs to be powdered as fine as possible to insure that the entire surface area comes into contact with the chemical in each step. any small chunks will hold gakk, crap, trash, heavy metals etc. DO NOT skip these fine sieve strainings where they are called for. a plastic sieve used for straining jellies is available in the canning section of most large stores that sell canning supplies and works the best. a small metal sieve can be used as well however metal is generally a no-no as the reaction with most chems with the metal is not a good one. if metal must be used make damn sure that what your passing thru it is bone dry 1st.
UPDATE
SWIM has taken to combining his 3 denat pulls into one jar instead of evapping them seperatley. SWIM adds the denat lets it settle out, siphons it off. adds denat to pill mass again, settles, siphons off, combines with 1st pull. repeats again. once 3 pulls have been collected in 1 jar SWIM then runs the 3 pulls thru fine filtration. SWIM`s fine filtration device is simply a HEET bottle with the bottom cut out and 6 or 8 cotton balls stuffed into the long heet bottle neck. SWIM packs them into the neck SUPER tight. SWIM uses a ringstand clamp clamped onto the heet bottle neck to hold it securley above the mason jar. if you just let it dangle in the jars mouth the long neck reachs almost to the bottom of the jar, you dont want this. so devise an apperattus to hold the HEET bottle. you can use a regular funnel if need be. a regular funnel is the originol way and works great but only holds a half cup of juice. SWIM likes his HEET bottle set up cuz he can pour in almost a pint of juice at once and walk away while it does its slow drip. in most cases SWIM only has to fill the inverted HEET bottle twice and all his juice is fine filtered. with the small regular funnel SWIM found himself having to fill it 8 or 10 times to get all the juice filtered. when all the juice from the 3 pulls has passed thru the fine filtration device then SWIM evaps it. scrapes up the crystals, makes sure they are totally dry, runs the crystals thru a fine sieve to powder them and then runs them thru the acetone wash. you will notice in most cases the tone takes on a blue green hue and the crystals are snow white. after a few min of being stirred in the acetone bath they are poured thru a single coffee filter. filter is wrung out and then crystals are spread on a plate to dry again. when dry SWIM again passes them thru a fine sieve to powder them, weighs them and at this point compares weight with what he should have gotten from the pill mass. if weight is far short SWIM does a 4th pull on the pill mass. if weight is within a couple grams or less from the expected return SWIM calls it good and chucks the pill mass. many say to save all these pill mass remainders untill several are saved up and then do a pull on them combined. SWIM says f**k that dont keep that shit around. its not worth this shit being found for a few grams of E. if the juice is at all cloudy pass it thru the fine filtration again. do it as many times as it takes untill it is clear as water. failure to do so will result in E that is unclean. if after two or 3 filterings it still has a cloudy look then pack more cotton balls in your filtration apperattus and make them tighter. when proper it should be a slow dripwith 1 or 2 seconds between drips. if it runs thru in a stream no matter how small its not packed tight enough.
there ya go young grasshoppers, another tidbit from the crew at upallnite productions & stucktomyshoe inc. to make your life a little bit easier.
remember this info is all hypothetical and was gathered from a dream state, compacted and found stuck to the dreamers shoe upon awakening. actual use of this info could land you in jail or worse.
************************************************** *********************************************
PART 3A: Acquiring I2 Crystals
I2 Crystals are available in several places however it is a very watched product. meaning it is tracked heavily by law enforcment. ordering it off the net etc. is very risky. do so at your own risk. when your setting in a prison cell with Ben Dover grinnin at you, remember SWIM warned you. what will be covered here is extracting your own I2 crystals from tincture.
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#5
 2008-11-15, 00:30
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
Last part of ephedrin, continued
NEEDED ITEMS: 1 pint 7% iodine tincture, 1 pint 3% hydrogen peroxide, 2 cups of distilled water, 1 ounce muriatic acid.
in a gallon jar (half gallon minimum) pour in the 7% iodine tincture, then pour in the 2 cups DH2O, stir it well. next pour in the 1 ounce of muriatic acid, stir it well. let it set for 15 minutes stirring every few minutes. now pour in 12 ounces (3/4 of the pint) of the hydrogen peroxide slowly while stirring. seal the jar. if the lid is metal place a plastic baggie over the jar opening before you screw on the lid. if you have no lid a baggie over the opening and a rubber band twisted tight around the neck will work. put it in a cool place that it wont be disturbed for 12 hours. after 12 hours you will see your crystals in the bottom of the jar. pour the liquid into a new jar add the remaing 4 ounces of peroxide and a capfull of muriatic acid seal the top again and put it away for another 12 hours. there will be another small batch of crystals to harvestfrom this. now take a gallon of DH2O and pour it in the jar with the crystals. pour the contents thru a funnel with a single coffee filter in it. it will drain slowly but patience is the key to success. when all the crystals are in the filter and the last of the liquid is drained pour in DH2O untill the funnell is full and let it drain. do this at least 4 times. SWIM does it 8 times. now take the wet crystals and filter out of the funnel, gentley squeeze out most of the water being careful not to tear the filter. at this point SWIM takes 10 paper towels and folds them in half, places the filter in them and folds them over the filter. he then presses the water out. when the paper towels are wet he repeats the process. when no more moisteure can be squeezed out this way he then places the filter in 1 paper towel closes it up and places it in a jar and pours damprid over the whole thing and lets it set 24 hours. when the crystals are removed from the damprid they are bone dry and ready to go into there storage container. SWIM recomends wearing gloves, chem goggles and working over wax paper. this will make cleanup a breeze.
so there it all is in a nutshell. if your after a quick easy way then you are in the wrong place. there is no quick easy way. if there was everyone and his brother would be doing it. the only quick easy way is to hit the street and buy the trashy cut shit you will find there. or take the time, learn the craft, and behold the best shit you have ever done with the pride of knowing you done it yourself. the game has its rules follow them and be rewarded. dont follow them and go to prison or the morgue or at the very least wind up with nothing,
hell these are possibilities even if you do follow the rules. remember that.
Ya got that under control? Well here is the rxn part of the deal.
ok here is how it goes... use the 1 part E, to 1.2 parts I2, to .8parts RP ratio for reactions under 1oz. So for example you would use 10g of E, 12g of I2, and 8g of RP. First take the RP and the E and mix well in a plastic baggie. Take this and pour it into your flask, covering the bottom of it.
Next pour in your I2 and close with a solid rubber stopper. Duct tape this on so it dont pop off during the reaction. you should all ready have your foot and a half of plastic tubing secured onto the nipple of the flask, and a pair of your chemical resistant gloves on. After you get the 3 goodies mixed in the bottom of the flask you will want to hold the end of the tubing closed with your thumb.(gloves on!)(safety glasses too)
Sit back and watch it start to react. Sometimes it will react right away and sometimes not. Just watch and see. It will start turning to a muddy texture, and then to a liquid. Every onece and a while release pressure in the flask by moving your thumb. now it will not always turn liquid before the cook. not totally liquid anyway. Just sit back releasing pressure when it gets great and wait for the reaction to really slow down.
All right, everything going good so far? Not too hard heh? Now you will want to cook the reaction to get it going again. Before you start all of this put your regular cooking pot on your electric burner and find out where the dial is at 150F. So turn on your burner and set it at 150F. Put your cooking pot with a little water or vegetable oil in the bottom on the burner, and put your flask in that. after a few minutes this bitch will really get cookin. It will start bubbling and the mixture will expand. All in all it is going to start to get a little crazy. Every few minutes pick up the flask and shake and stir it up a little. And usually release a little pressure every shake or every other shake. You will be able to feel the pressure building up on your thumb. When it gets bad release a little.
Just keep this going for while. You will want to slowly turn up the heat to about 180F over a 20 minute period. The push part of the reaction will keep going for about 20 minutes to 45 minutes. It usually lasted for about half an hour in my dreams. You will know when to stop cooking when the push stops. (when no more gas is being pushed out of the flask.
When this has occured be sure to keep your thunb over the tubing and take the flask out of the pot and just set it on the counter. From this point on, you are going to keep your thumb tightly over the tubing until the flask has cooled down. During the cooling you want to pick up the flask with your other hand and stir and shake the ingredients in the flask every few minutes.
It will probaly take about 20 minutes (if that) for the flask to cool down. You want it to be cool enough to hold in your hand with out burning yourself. You will feel the pull start as your vessel cools down. it will be trying to suck air back into the flask now. You are aloud a very little bit of air into the flask but not much at all. Remember to keep stirring and shaking the flask during the cooling.
When the flask has cooled down to a suitable state, (keeping your thumb over the tubing still) stick your thumb and the end of the tubing into a bowl of distilled H20 and release. The vacuum in the flask will pull water into the flask. Dont let to much into the flask just a little. now pull the tubing out of the water and let it suck air into the tubing. Thats it. thats the reaction. not to hard hey? Now lets clean up that chilli. All ready smelling success? wait and see
Shake up the chilli/H20 in the flask, take off the duct tape and the stopper, and pour directly into the clean visionware bowl. now pour a little more distilled water into empty flask (just a little) and shake up real good. this is just to get out the rest of what ever is left in the flask. put the bowl on the burner and turn on high. bring to a boil while stirring with a clean plastic spoon. This will get the some chilli that is stuck on the RP off of it. turn of burner and let sit for a minute or two. be sure to save all your RP so you can wash it and reuse it later.
While this is cooling off a little, grab your funnel and put in 3 coffee filters and stuff a cotton ball in the tip of the funnel. put this over a clean glass jar. now pour everything that is in the visionware bowl into the funnel. it will take a while to filter because of the RP. once all the meth water is filtered through, into the glass jar, pour it back through the same filters (with the RP in it) again. you will want to do this at least 4 times. just keep pouring it through the same filter/cottonballs. now it should have a yellowish collor, but not foggy at all. it should be very clear.
Pour this into your separatory funnel, and add just a little ice. now pour in a little colemans fuel (or toluene). add a little less than the amount of water/meth you have in there. now slowly add a little lye to the sep. funnel, and shake well. drop a small drip onto your litmus paper to test the Ph. (you will be testing the water/meth layer, NOT the colemans fuel layer) you want the Ph to be 12. (yellow) if it is not a Ph of 12 then add a little more lye and shake the hell out of it and test again. keep doing this till it test out at 12. After it test at 12 drop in a tablespoon of table salt, and shake well. Now we are going to seperate the layers in the funnel. We want to keep the NP Solvent (Colemans), not the water/lye layer.
Put the water layer in a jar and set aside. you can test for meth later. Keep the colemans fuel/meth in the seperatory funnel. microwave a big glass of new distilled H2O till it is hot. pour in one third the amount of water (compared to the colemans) and shake well. drain the water out. repeat this 4 times. you are washing the NP Solvent. now once again, add one third the amount of water to the sep. funnel and drop in a few drops of Hcl. (Muriatic Acid) Shake for a few minutes. then test the ph of the ph of the water layer. you want it to test at 7.2 or at least close to that. if it doesnt, add a few more drops of Hcl and shake the hell out of it again and test again. after it is the proper ph, drain the water layer into your visionware bowl and put it on the burner and boil down. you can finish with a hairdryer if you want. now go back to your colemans fuel in the seperatory funnel and add a little more distilled water. we are going to do a second pull on the non-polar solvent. add a few more drops of Hcl and shake it up again. test the ph again. looking for 7.2 again. once you reach 7.2 again drain your meth/water into your clean visionware bowl (you should have all ready scraped out the crystals from the last pull that you all ready evaporated. now evaporate again. remember that if your not in a hurry, evaporating it with a hair dryer will increase yeilds. Some chefs even do a third pull.
Thats it. you now have clean and pure crystal meth. Have Fun, and be safe.
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#6
 2008-11-15, 00:38
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
MDMA synthesis from MDP2P
Preparation of MDMA via. Sodium Borohydride
By: Cure20
Ok first I would like to say that credit is deserved to those key players that helped me out a lot at www.dr**s-forum.com. You know who you are and I appreciate your help. Secondly I could not get anywhere without the help from the report written by LabTOP. My main goal in writing this is to help those first time people out there that are going to attempt this but need step by step instructions as well as a good visual. Some of the reports out there that I have read I have noticed that all the materials needed and the procedure are all in order but as far as the minor details such as color, sound, taste(just kidding about that one) etc. I remember my first dream, very stressful, asking myself hundreds of questions over and over again Was that supposed to happen? Is it supposed to look like that? Is it supposed to be making that sound?
Anyone been in this position, its a little nerve racking because you dont want to mess it up, but let me tell you nothing feels better then that feeling you get when you see those first little bits of MDMA.hcl precipitate and a big feeling a relief comes over you. If you follow this step by step I promise it will work for you in yields reaching some where in the high 90s on the first pull, but somw will be lost in the recrystalization.
Ingredients
- 500g of MDP-2-P *chilled in freezer*
- 1500ml of Methanol *chilled in freezer*
- 150g of Methylamine gas
- 50g of Sodium Borohydride(NaBH4)
- 500ml Toluene (DCM can be used as an alt.)
- 2000ml Acetone
- 2 Bags of ice
Equipment
- 4L beaker or anything that is HDPE (High Density Poly Ethylene) eg. Bucket, Tupperware container
- Stir plate with stir rod
- Thermometer
- Distil Setup (*optional*)
- Sep Funnel
- Scale that can weight up to at least 3000g/3k
Preparation Step
150g Methylamine gas into methanol
- This procedure involves making a 10% methylamine in methanol solution, by bubbling the methylamine gas into the methanol allowing the cold methanol to catch the gas and changing it to a liquid and allowing to settle in the methanol.
First attach a thick black rubber hose to the methylamine gas tank valve, making sure no pressure regulator is attached, allowing enough length for the tank to be upside down at a 45`degree angle and allowing the hose to be able to reach the bottom of the vessel that going to have the methanol in it.
Next youre going to place the 1.5L of ice cold methanol, which was left in the freezer overnight, into any kind of vessel that is at least 2 liters such as a flask, bottle, just about anything that has a small mouth so a damp paper towel can cover it up. Pre weigh the flask with the methanol in it and mark it down on a piece of paper so you dont forget it. So lets say that your total weight was 2000 grams, then that would mean that your target weight would be 2150g. Now place the rubber hose in the methanol allowing hose to go all the way to the bottom then place a damp paper towel around any openings that might expel any gas. The paper towel doesnt have to be too wet just enough to absorb small amount of gas that might leak out of the methanol. (Keep in mind 1000ml of h2o can absorb 1000g of methylamine gas)
Now your going to want to bubble the methylamine gas into the methanol by opening the valve on the tank *slowly* until it start bubble a fair amount. Stop the bubbling and weigh the vessel until you have reached the desired weight, I like to weigh it every 2 minutes or so. This should take about 15 minutes and when done close off vessel with plastic wrap and chill in freezer for about half an hour because bubbling the gas into the methanol make it warm up a fair bit, and besides it going to take you a bit to prepare the next step.
SAFTY TIPS:
-Dont open the tank up too far because the vibration alone will force the vessel to fall or tip over.
-ALWAYS* close the valve fast because there will be a pressure change and this will cause the methanol to be sucked up the hose and into the tank. If this happens it could cause the tank to rupture and explode right in front of you.
-Try not to wear a mask because if there is a gas leak it can be smelled thus avoided. If wearing a mask you might not be able to smell it and it can be absorbed by the skin.
Preparation Step (2)
Take the 4L beaker and place it on an ice bath on top of the stir plate. Pour in the 500g of chilled MDP-2-P and turn the stir on. Now pour in the 10% methylamine in methanol solution and allow to stir for five minutes. Solution should now be a little orangeish. If both MDP-2-P and methanol were chilled long enough then temperature should be about 5`C. If it is not and it is around 10 15`C the allow to stir for 15 minutes until it reaches 5`C.
- After adding the methanol solution to the MDP-2-P a desiccant such as Silica Gel can be added to remove any water formed but this is unnecessary because the amine is a lot more stable then P-2-P. The idea behind that is that not removing the water causes the water to eat up the NaBH4 instead of the reaction happening but this is not true with MDP-2-P. So adding a desiccant only helps later when you need to distil any water and methanol from the oil.
- adding regular table salt and a bit of acetone to the ice bath keeps the ice from melting fast, and keeps the bath colder longer before having to add more.
Addition of Sodium Borohydride
Now that you are confident that it has reached 5 C it is time to add the NaBH4. Now the idea here is to add the Sodium one tea-spoon at a time every five minutes with stirring. But for your first addition I would suggest that you add a half a tea-spoon just to get the idea of what is going to happen here. When you add the sodium it creates a fair amout of H2 gas and fizzes quite a bit so take my suggestion because the first time can scare the shit out of you with a full spoonful (Trust me)
With each addition the temperature rises a fair bit so you wanna keep the temperature around 8 C before adding more. As well with each addition your going to have to wait for the H2 fizzing to die down before adding more. It doesnt have to die down completely but enough so if you were looking from above, you can at least see the stir rod spinning again. After around 4 hours all of the NaBH4 should be added. Take the beaker out of ice bath and put paper towel over the top with a little plastic wrap to hold in place. Put back on stir plate and allow to stir for 20 hours.
TIPS:
- Some may say closing off the vessel and having a small tube exaust out the window. But working under a fumehood or having a fan blow towards the vessel out a windows is just fine. It states that having a open surface area causes oxidization but that was belivied to affect the P-2-P to Meth process. This one is more stable as mentioned earlier.
- You will notice that close to the end of addition fizzing take longer to die down but just be patient you dont want to fuck it up.
- If water was not remove with a desiccant then fizzing will come to a complete stop. If water was remove with desiccant then fizzing will almost never stop at which point just time the addition for every 5 minutes.
After everything was allowed to react for 20 hours, Contents were poured off into a sep. funnel and 4L of water was added and allowed to separate for 30 minutes. When water is first added the entire solution is milky white, but after a minute or so you will notice the oil beginning to separate at the bottom and the water should be clear after time duration of 30 min.
Next drain off the bottom oil layer into a clean 4L beaker and put aside some place safe. Take 200ml of Toluene and pour it into the sep. funnel and shake for about a minute or so (remember to let the pressure build up inside the sep. funnel to be released)
The reason for this is to allow any left over oil that hasent been separated out of the water to be sucked up into the toluene. Now drain off the bottom water layer and put aside, you dont have to throw water away because it can always be used for the next batch. Add Toluene/oil to the rest of the oil in the 4L beaker, volume should be approx. 800ml. Now go and prepare your distillation setup.
TIP
- After reaction is finished all the methanol can be distilled off instead of adding the 4L of water which is fine for this batch but if one was to upscale to a size around 5L of MDP-2-P, then distilling off 15L of methanol would be a pain in the ass as well as being more time consuming.
Distillation
After your distillation setup is prepared. Pour in your oil/touluene solution into the boiling flask and begin to distil at atmospheric pressure. First the methanol, Toluene, water and other low boiling stuff are removed. The water and other low boiling stuff comes over at 130 C. When this is done and nothing more is dripping over into the receiving flask, remove it and replace with a new clean one. Apply the aspirator or other vacuum source and allow vacuum to build. At first around 140-145°C you see the first little drops of oil condensate and at 160-165 C it starts Running.
When freebase oil stops dripping and the tempature begin to drop, turn everything off and allow to cool for an hour. The reason I say an hour is because it is probably best to clean you boiling flask with hot water while the leftover garbage is still warm because if that shit is allowed to cool it is a bitch to get clean.
TIP:
- Some people say that the use of an aspirator is not sufficient enough to distil the freebase oil and that a good vacuum pump is recommended but I have done just fine with one for a little batch like this, anything above then I would recommend a vacuum pump.
Crystalization
Mix your freebase oil with clean and cold acetone that was chilled overnight in the freezer, and bubble through with a Stainless steel pipe 8 mm x 1 meter with HCl-gas SLOWLY! After about 5 min a thick, white crystal mass will form and sink to the bottom. Check frequently with pH-meter or paper until pH reaches 7. If the solution gets too hot then place in the freezer for 20 minutes be careful not to go under pH 7 to 6,5, because then your powder will solute again and you must add base again until pH comes up again to 7. So keep at least 20 ml of base ready in case of a mistake. Filter off the acetone/powder mix in a funnel with aspirator vacuum then dry the powder on glass plates
TIP:
- If you dont want to gas then adding straight muriatic acid to it can also be done. But your going to have to remove the acetone and water with another distillation. When all the water is removed, the oil doesnt flash into a powder, it gets real thick like tree sap, then begins to harden after heat is shut off and allowed to cool. If you do take this route, then please pour hot oil into a glass baking plate before it gets a chance to cool because it get hard like a rock and it is damn near impassible it get out of a round bottom flask without extremely damaging your final yield.
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#7
 2008-11-15, 00:44
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PandaOfAMan 
Regular
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Re: BLTC Home Ec - Food for Thought
fail5
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#8
 2008-11-15, 00:46
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
MDMA from sassafras oil synthesis
1. Distillation of sassafras oil
First of all I m going to tell you if you would want to make MDMA you would need a source of safrole, you could get this from a chemical company or distill it out of sassafras oil.
Via the chemical company is not an option for 99/100 people so that s why I m going to tell you how to distill it out of sassafras oil.
Sassafras oil itself is even hard to get by, but after searching for very very very long you will eventually find it hopefully.
I m not going to tell you where to find it or how to find it, just only use this book when you already have a bottle of sassafras oil lying around.
Well to the distilling now. In the picture below you can see a distillation setup, there is no vacuum used when distilling safrole this worked out just fine.
Pour the sassafras oil in the distillation flask, and put the flask in a heating mantle or another heating source.
Here below you can see a bottle of sassafras oil and a distillation setup which is distilling sassafras oil.
On the bottom left you can see the heating mantle it is also covered on top with alluminiumfoil, to prevent a lot of heat to escape.
The whole vigreux colomn is also packed with alluminiumfoil on the outside, else the heat will not propogate to the thermometer and the distilling head.
The thicker glass tube you see standing slope is the cooler, ICE cold water is floating threw the double glass wall, and threw the glass spiral, this is to make the evaporated safrole condensate again.
The vigreux colomn is used to get a more pure product, and it also is nice to be there, because when distilling the oil it, the oil will bump very hard in the flask. It might even scare you the first time.
It needs to be 230*C in the top of the distilling head, it is suggested to use boiling stones in the flask to calm the bumping down a bit.
Do not close the setup completely else there will be too much pressure inside, as you can see on the right of the picture there is another flask and on top of that flask there is a piece of glass which is bent it is called an allonge it has an vacuum adapter piece to it.
If you do have a vacuum source you can connect your vacuum tube to that piece of glass. Now it functions as a pressure release opening.
Here you can see the temperature going over 200*C.
Here you can see the pure safrole in the flask which came over, it is water-white oil.
Out of 90ml sassafras oil, 75ml of safrole is distilled out. On the right you see the tar and rest of the crap that is left in the distillation flask, this stuff doesn t come over so apparently it will be a chemical that wil have a boiling point greater than 300*C.
2. Isomerization
Now that we have the pure safrole, we can start with the next step. Isomerizing the safrole to isosafrole.
Safrole itself looks like this
Many ways of isomerizing safrole (3,4-Methylenedioxyallylbenzene) into isosafrole (3,4-Methylenedioxy- propenylbenzene) can be found in the literature. The isomerizations, which in all reviewed cases are catalytic, often have high yields, but differs greatly in easiness and reaction times.
The availability and costs of the catalysts also differ over a broad range.
The reaction, which is general for the conversion of nearly all allylbenzenes (like safrole, apiole, dillapiole and elemicin) to their corresponding propenylbenzene isomer, is usually carried out by heating the allylbenzene together with an inorganic catalyst or catalyst mixture under reflux, with or without the use of a solvent. After the reaction is finished, the catalyst is removed by filtration, any solvent removed under vacuum, and the residue is distilled to purify the propenylbenzene from unreacted allylbenzene and polymerized material.
Glassware set up for reflux.
Reflux means that the cooler is put inside the flask upside down, and so when there are chemicals in the flask that can evaporate easily they would normally evaporate and be gone out of the reaction when you heat it to let them react.
If you would place a cooler on top of the flask the chemicals which evaporate will cool down again and fall back down in the reaction flask.
That is in short the principle of refluxing.
The person who did this synthese let s call him SWIM poured the 75ml safrole in the flask. He added to this 30ml 96% ethanol and 21,10g of KOH.
SWIM refluxed it for 3-4 hours on a gentle reflux of 60*C.
After adding the KOH to the safrole+ethanol the mixture turned brown.
Toluene is poured into the sludge which remains and threw the filter to get all the isosafrole out of there.
Toluene doesn't mix with water, it has a lower density (0,86g/ml) so it floats on top of water.
Drain of the water layer, and keep the toluene layer, add this to the filtrate and distill it to get rid of the red/brown color, but before you distill it you need to neutralise the KOH with an acid, SWIM used H2SO4 diluted in water to 50% and checked it with pH paper to get it only a little bit basic.
This is what is left after distilling the isosafrole, the yield was 80% by weight. It was 66ml.
3. Epoxidation reaction via peracetic acid
First of all you need DCM (dichloromethane aka methylenechloride) it is sold as paintstripper and as brush dehardener.
In the country where SWIM lives they only sell paint stripper with a wax binder which sucks, so he found that the brush de-hardener didn t contain any wax binder so he distilled the brush de-hardener.
It contains: DCM, methanol, solvent-naphta, hydrogenated naptha.
Both the naptha s have a boiling point greater than 100*C, the methanol 65*C and the DCM 39-40*C.
So without a vigreux colomn he distilled the DCM and it came over at 39*C until 41*C.
The mixture itself was 55*C and the gastemperature was 39*C and at the end 41*C the mixture contained 65% DCM.
The addition funnel is to get the DCM in the 1 liter round bottom flask.
All the DCM is added to the flask (500ml) and it is ready for the heating, so SWIM turned on the heat and started to distill of the DCM.
To do the peracetic acid epoxidation reaction, the isosafrole needs to be dissolved in a solvent to make it mix with the peracid, alcohol can be used but due to alcohol containing water easily it is not a good choice. Acetone is also quite a lot used but SWIM didn t want to use it because you need to distill the mixture after you are done with the MDP2P reaction.
And acetone can form acetone peroxide with hydrogen peroxide and an acid (acts as an catalyst).
Acetoneperoxide is a high explosive, which detonates from heat.
So guess what happens if you used a bit too much H2O2, and then you are going to distill that mixture Acetoneperoxide are white needle like crystals by the way.
Anyway to make the peracid one should do the following:
Pour:
- 55,8ml of 99-100% glacial acetic acid
- 55,2 ml hydrogenperoxide 35%
- 0,66 ml sulfuric acid 96%
All together in a flask, let this react for 4 days, it doesn t heat up, just stink like acetic acid very badly. And let it react for 4 days to get to it s equilibrium, and then it can be used.
Dissolve 33ml of isosafrole in 51ml DCM.
Add this slowely to the peracetic acid, and let the temperature not rise over 40*C. You should place the flask on a magnetic stirrer in an icebath while doing this.
After everything is added, let the ice-bath come to roomtemperature by itself, and leave it to stirr overnight, with some foil over the top of the flask.
The color will go from yellow to orange to deep red, distill of the DCM and distill of the acetic acid. A dark thick syrup will remain.
Dissolve this syrup in 51ml methanol and add to this 250ml 15% H2SO4 solution. Let this reflux mildly for 3 hours.
Then when it has come to room temperature drain off the acid layer, and keep the dark layer. Pour the dark layer in 125ml of water and then extract the syrup again.
Then wash it with 125ml of NaOH solution of 5%, this last wash is difficult to see so use a flash light to see where the phases separate.
Now pour in 5g of MgSO4 (epsomsalt) which is completely dry, dried in oven at 300*C for 4 hours. Filter of the MgSO4 again and wash the MgSO4 with DCM.
Distill the resulting liquid, this is your pure ketone.
Here you can see 51ml of dichloromethane mixed with 33ml of safrole, it does not mix when just poured onto each other,
SWIM sucked the mixture up with his pipette and blew it back in the rest of the liquid to mix it, until it was mixed well, it was quite easy to mix.
Here you can see the icebath with the isosafrole and DCM mixed in there, while the peracetic acid is being added to it slowly.
As you can see it is in an icebath as mentioned above, this is to prevent the liquid becoming to hot, and get to a boil.
Although it should not exceed 40*C, DCM is used as a solvent so you also need not worry about explosives peroxides(since you need to distill this mixture) when using acetone make sure you do not add too much H2O2 since if not everything is used up by the acid it will peroxidize your solvent if it is peroxidizable (such as ether and acetone).
you can see the color change, the first picture is after everything is just added, the 2nd after an hour and the third after 2 hours and so on, on the third it is capped with Al foil, and left to stir for 16 hours.
As you can see the color changes from clear to yellow to orange to red to dark black-red.
Now the 16 hours has passed it is time for the DCM to be distilled off.
Thus SWIM poured his mixture in another round bottom flask and set it up for distillation
Now it is time to get rid of the acid, that is done by adding NaOH solution SWIM used around 3g of NaOH in 150ml water, and used it all to neutralise the peracetic acid he made. Below you can see pictures of a wash with ether after it was neutralized, this was done twice
You can see the layers quite badly, although you can see an upper layer which is slightly darker then the other layer, ether will float on top since the density is a lot lower then that of water.
The ether is distilled of at 39*C, and pure isosafrole glycol is what you have in the flask then. This needs to be turned into MDP2P you can see the reaction mechanism below.
You need to pour as much methanol together with the isosafrole glycol as you used solvent for the isosafrole.
In SWIM s case that was 51ml so now he uses 51ml methanol to dissolve the isosafrole glycol in, and add s 255ml (5 times as much as the methanol) 15% H2SO4 to it.
If you take 99% sulfuric acid, that is the most common to buy as draincleaner, one could also buy battery
acid. That is 37,5% sulfuric acid, dilute it 2,5 times with water to get 15%, but if you couldn t figure that
out, you didn t get this far with the synthese although you should read this whole thing before beginning
anyway.
When using 99% you need to dilute it 6,6 times.
When using 96% (also quite common instead of 99% as draincleaner) you need to dilute 6,4 times.
The density of H2SO4 when concentrated is 1,84g/ml, so you need 1,84g with 6,4 times as much water. 1,84g*6,4g = 11,78g water. 11,78g/0,998g/ml = 11,80ml water.
1,84g = 1 ml
So for every milliliter H2SO4 you need 11,80ml water.
You need 255ml sulfuric acid, 255/11,80ml = 21,61 ((19,92*11,80)/0,998)= 234,53 ml = 234,06g
((19,92* 1,84)/1,84) = 19,91 ml = 36,63g
234,06g / 36,63g = 6,4 times as much
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#9
 2008-11-15, 00:50
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
Continued
This is what it looks like just plain, not with a lamp underneath it, this is only the first wash by the way. The next wash will be added to this, and then the ether is distilled of and the pure isosafrole glycol
remains and then you should add the methanol and the sulfuric acid. (mix the sulfuric acid ahead with
water).
Reflux this mixture for 3 hours and no longer else the yield will go down, now you have raw MDP2P.
Now let it cool down to ROOM temperature, now pour off as much as water as possible, and pour new
fresh water in there so the flask is filled half or 2/3th and mix well, and let the layers separate and decant of the water.
Do this 4 times, this should be good enough to remove the last traces of sulfuric acid left in the oil.
Now for the last time adding water decant off the water, and attach a distill head etc. onto the flask, and
start to distill the MDP2P.
From another synthese I read the MDP2P comes over as a yellow to brown oil at 115-170*C with a
aspirator vacuum, and then redistillation gives yellow oil (MDP2P) at 140-150*C.
At SWIM the MDP2P came over at 158°C with vacuum, SWIM collected 15g of MDP2P that is a yield of +/- 45% which was yellow golden in color and when held against the sunlight it has a greenish look from some sides depends on how one looks at it.
Another method to collect your MDP2P would be (and also to test if it is real MDP2P) with sodiumbisulfite.
One would make an saturated solution of sodiumbisulfite, and drop a bit of what should be MDP2P into it,
and if a preticipate forms, it is a ketone, and most likely MDP2P, since it just happens to be a ketone
It is a somewhat well known fact that sodium bisulfite will add to the carbonyl group of a ketone to form a crystalline addition product. If the parent ketone is of large enough molecular weight, the product will be insoluble in water. The parent ketone can then be recovered at a later time by decomposition with sodium hydroxide. This is a doubly good trick in that it gives us an excellent way to get pure ketone from an
impure reaction matrix and it also allows the long term storage of an otherwise unstable ketone prior to its use.
Now, this doesn't *eliminate* the need for a proper (vacuum) distillation of the ketone, but it does make
such a process much more pleasant in that when recovering from the bisulfite, there will be little tar and/or
polymerized crap to deal with. This means greatly reduced cleaning for those precious flasks, and,
possibly, higher yields.
The bisulfite addition is a fairly general process, and may be adapted to many
different ketones (keeping the molar ratios in proportion), however, there are going to be some ketones
which will either not react or react to a low extent (mainly ones in which there is significant steric
hindrance to the carbonyl carbon). In cases where the carbonyl carbon is on an aliphatic side chain to
some other funky ring structure, there is little steric hindrance, and so the reaction proceeds quickly and
nearly quantitatively. Finally, there is the limitation that that ketone (or ketone containing slop) be reasonably free of acidic or basic impurities, as these will interfere with the formation of the addition
product.
1) Preparation of the bisulfite reagent
(This must be prepared just prior to use, as it will autooxidize within hours if left to it's own devices.)
Add 52g sodium bisulfite (NaHSO3, .5moles) to approximately 90mL of distilled water at room
temperature with vigorous stirring (slightly more water may be used to get it all into solution). Add a volume of denatured alcohol of about 70% of the solution's volume (ie - if you end up with 100mL of solution, add 70mL of alcohol) then add more water to just dissolve the precipitate (~60mL).
2) Reacting with the ketone
Slowly drip .25moles of ketone(*) into a beaker containing the bisulfite solution with vigorous magnetic stirring. The 2:1 molar ratio insures that all of the ketone will be converted. Let sit on the stirrer for an additional 30-45 minutes then filter on a vacuum Buchner funnel. Wash the crystals with 20-50mL of denatured alcohol. Dry in a vacuum dessicator or open tray then store in a stoppered glass bottle until
needed.
(*) If adding an impure reaction matrix, add as much solution as you expect to contain .25moles of ketone.
3) Recovering the ketone
Add the ~.25moles of bisulfite addition product to a separatory funnel then slowly pour in 105mL of 10% Sodium Hydroxide solution (w/w). Separate out the aqueous layer (which may be on top or on bottom depending on the ketone), saturate with salt (NaCl), and extract with 50mL of ether (toluene or benzene ok if the ketone is of high enough bp). Combine the extract with the ketone layer and strip off the ketone by distillation (condense and reuse!). Distill the ketone residue, preferably under vacuum (if you're making what I think you're making), to yield up to 90%, depending on the purity of the starting ketone, of course.
Refs to chase: A. Vogel, "Practical Organic Chemistry"
Now one has MDP2P if one wants to store it do so in the freezer it will become a very viscous liquid and
will be storable for LONG times.
Now will be outlined how MDP2P can be synthesized with the wacker oxidation and p-benzoquinone a la Methylman.
4. p-Benzoquinone Wacker oxidation.
To convert safrole to MDP2P one does the following:
- Distilled sassafras oil to yield safrole 18ml
- 40ml MeOH
- 0,2g PdCl2
- 5ml dH2O
- 15g p-benzoquinone
First let all the chemicals stirr for an hour exept for the safrole, the safrole has to be added later on after everything has been mixed thorougly for an hour.
Then start dripping in the safrole this should take at least an hour, when dripping is at 80% then start heating slowely and after everything has been added start a reflux for 8 hours.
After the 8 hours have passed, throw the whole reaction mixture threw an buchner filter to filter out any residue like hydroquinone (degradation product of 1,4-benzoquinone) and PdCl2 (don t try to recover this it is not worthwhile).
After filtration add 150ml 10% HCl to hydrolyse the reaction to MDP2P stirr for 15 minutes and
now extract 3 times with 100ml DCM, 50ml and 25ml DCM.
Combine extracts and wash them 2 times with 50ml saturated sodiumbicarbonate solution, then 2 times with 50ml saturated NaCl solution.
Then wash the extracts which have now turned color a bit more greenish/yellow with 5-10% NaOH solution and do this 3 times with a volume of 100ml per wash, now dry the ketone after the NaOH solution has been drained off with MgSO4 or Na2SO4 (anhydrous).
And after it has been dried distill of or rotavap off the DCM and be left with impure MDP2P.
This needs to be distilled and there are a few pictures of below:
I ve heard it smells like flowers but I don t think it does it doesn t even smell nice it doesn t stink but well it s like safrole a bit but then a bit more like flowers then safrole, but not really like flowers well anyway smell it when you made it and you know. It has a greenish hue on it.
This is the reduction setup, but the same is the wacker oxidation since there is the safrole on the
right and on the left the condenser for reflux and an overhead stirrer in the middle a heating mantle in the middle too, and in the back a bucket with 10 liters of cooling water.
After the MDP2P has distilled one will have around 8ml MDP2P to 15ml.
SWIM got 8ml it was the first time doing this reaction but the yield will go up with more experience probably.
5. Reductive Amination MDP2P to MDMA freebase.
First 4ml MDP2P was reduced in a 500ml round bottom flask with 8g of Al foil which has been
put in the coffeebean grinder before and overhead stirring used etc exactly like the picture above.
Enough MeOH was used to cover the Al and 60mg HgCl2 was dissolved in 20ml MeOH and added at once to the reaction threw the dropping funnel, then after 15-20 minutes the
amalgamation started, small bubbles occurred and then bigger ones which is the point where the MDP2P needs to be added but since the MDP2P IF you will reduce it as it is will only yield MDA (in acidic conditions) we want MDMA so we add nitromethane (which will be reduced to methylamine in situ) and that forms an imine which then will be reduced to MDMA.
This is an BASIC Al/Hg reduction (reductive amination), when reducing nitropropene s or styrene s then an acidic Al/Hg reduction is used with addition of example glacial acetic acid.
Methylamine is alkaline and will thus make the reaction basic.
Reduction going, make sure to add the MDP2P+MeNO2 at one drop per second if you will drop everything in there at once one will get a very vigorous reaction and you will get drained in
boling MeOH and mercury etc not very plesant.
So use 4ml MDP2P and 3,3ml MeNO2 and 8ml MeOH in the dropping funnel.
Look at the foam this is how heavy the reaction is, here the Al is dissolving in the MeOH due to the HgCl2 while it does this it reduces the N-Methyl-MDP2P imine to MDMA.
When the reaction will cool down again then add the MDP2P+MeNO2 faster if you ran out of MDP2P+MeNO2 then start heating and reflux until you reached 3 hours.
After 3 hours add NaOH solution (concentrated) and this is for the Al that hasn t dissolved so which is left in the flask, this will heat up too and make the MeOH boil, anyway don t add the NaOH too quick since then there it will also foam and then it could also come out of the
condenser.
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#10
 2008-11-15, 00:50
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Re: BLTC Home Ec - Food for Thought
Lab tips
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#11
 2008-11-15, 00:51
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The Exile 
Regular
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Re: BLTC Home Ec - Food for Thought
continued
So after the addition of the NaOH let it stir for 1 hour to make sure everything dissolved.
Now you will have 2 layers a bottom layer with Al(OH)3 and probably black and an
orange/yellow/red aquous layer this it the layer you want filtrate off the Al(OH)3 in a buchner
(needs to be vacuum), and then one will have something like this:
The filter, you might need to do the filtration in part since the filter will clog up pretty much and even with strong vacuum you can't get it threw anymore.
Anyway first evaporate the MeOH from the reaction then extract the remaining liquid with DCM 3 times (or any other non-polar solvent) SWIM just loves DCM since it rotavaps off really quick .anyway.
Then evaporate the DCM, then do an a/b or distill the MDMA freebase, SWIM normally prefers distillation but one needs a vacuum pump which can pull below 10mbar for this job else the MDMA oil will decompose so aspirator won't do.
Use the acid/base extraction, if you don't know what that is you shouldn't be doing this synthesis.
In short the MDMA oil can be an oil or an salt, the salt is water soluble and the oil isn't.
You take advantage of this, right after the reaction when the oil is in the DCM, wash the DCM with water and NaCl solution and NaHCO3 solution, this takes out all the crap that does dissolve in water.
Then add H2SO4 to the oil after DCM evaporation (since then you see how much impure MDMA freebase you have) then add twice as much molar H2SO4 solution like 5%-15% solution, then add DCM and you can extract all the crap that does dissolve in non-polar solvents once again here you can also use chloroform or toluene etc.
Now add NaOH to the water layer and do this with a NOT concentrated solution of NaOH.
Then you will see some white stuff when adding a bit of NaOH solution, this actually is the MDMA freebase which if you leave it will settle to an oil layer on top of the water, but just do this and shake until the white cloudiness persist (means it doesn' t go away anymore) then add DCM and add more and shake everytime after every addition of 1-3ml and then when no more white cloudiness forms add the rest of the NaOH solution at once until pH = 12-14.
Then drain off the DCM keep it and extract the now basic aquous mixture with 2 times more DCM and combine, evaporate DCM and you have pure MDMA freebase.
6. Crystalization of MDMA freebase to MDMA.HCl
4,0ml MDP2P yields with this method 3,0ml exact MDMA freebase, which needs 1,95ml of 29% HCl solution or 0,566g HCl calculate your own amount for your concentration you have.
Just add the HCl solution while the freebase is dissolved in toluene (dry).
Now you will have an little aquous layer on the bottom of your little RBF, now put a dean&stark trap on top of the RBF or just attach it to a distillation setup, the point here is to distill of the water, the dean&stark trap breaks the azeotrope which normally is formed with water and thus drives off the water, anyway when the water evaporates the HCl salt of MDMA will then settle out as a brown paste or very viscous layer on the bottom.
Then after all the water and some toluene came over you add the double volume of acetone so for 3,0ml MDMA freebase you use 10ml toluene and 30ml acetone (anhydrous) this sucks up the water that still is in there, and then the paste will turn into nice white crystals (the acetone also takes up some crap).
Now put in freezer overnight or couple of hours and filtrate and wash with acetone (anhydrous and cold).
Tadaaa 3000 mg MDMA HCl.
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#12
 2008-11-15, 02:59
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Re: BLTC Home Ec - Food for Thought
Lab tips
No NOT lab tips idiot. This kind of shit doesn't go anywhere. OP, what is your point? You just posted a bunch of random copy paste shit. Do you have questions? Because discussion about chemistry doesn't even go here, and lab tips has no use for your copy paste bullshit.
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#13
 2008-11-15, 03:46
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Dmt_Tengu 
Regular
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Re: BLTC Home Ec - Food for Thought
first of all 99% of people here aren't going to understand that shit, secondly for all i know you're a fed , lastly I think it's safe to say people already got their own recipes .
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#14
 2008-11-15, 04:57
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Re: BLTC Home Ec - Food for Thought
Phenyl-2-Propane
http://img530.imageshack.us/img530/8315/p2ptypowq3.png
Please correct basic chemistry errors if you are going to copypasta.
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#15
 2008-11-15, 08:42
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Re: BLTC Home Ec - Food for Thought
tl;dr
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#16
 2008-11-15, 16:24
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stateofhack 
Regular
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Re: BLTC Home Ec - Food for Thought
http://img530.imageshack.us/img530/8315/p2ptypowq3.png
Please correct basic chemistry errors if you are going to copypasta.
This and your P2P synthesis is shit old, get over is there are better ways.
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#17
 2008-11-15, 19:10
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incorporated 
Regular
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Re: BLTC Home Ec - Food for Thought
If you were going to do this intelligently, you would have just c/p'd the LINKS from the websites you took all that shit from. It would have taken less space, looked a lot cleaner but still been just as useless.
Just stop.
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#18
 2008-11-15, 20:36
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ShroomLove 
Regular
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Re: BLTC Home Ec - Food for Thought
No NOT lab tips idiot. This kind of shit doesn't go anywhere. OP, what is your point? You just posted a bunch of random copy paste shit. Do you have questions? Because discussion about chemistry doesn't even go here, and lab tips has no use for your copy paste bullshit.
This. 
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