Man, what a holiday it's been!

Finally, got some free jacked up time to post some write-ups like SWIM has promised. SWIM still isn't done with the whole process. Had to stop due to holidays, plus had some company for a few days. So SWIM didn't get to work on shit since he's been back. Gonna start building that tube furnace tonight though.

Alright where should SWIM start? First off, SWIM wants to say that so far every procedure he's done has been totally easy. It may have required a few hours of hard work and some four letter words when fighting with the apparatus during the glassware balancing act, but other than that it's pretty simple and easy.

First step:

Toluene----->Benzyl Chloride

SWIM had wanted to use LiOCl as chlorinating agent, as yeilds would have been so much higher, and this would be so much easier. Due to lack of money and transportation (plus all major pool stores were closed, and SWIM was like "fuck it" cuase he was on a time schedule) he couldn't get any. So the classic chlorine synthesis was performed.

Chlorine reacts with toluene, forming benzyl chloride and HCl. Now SWIM did this in a room that was not really lit up at all

(actually it was kinda dark), and it was night time. Traditionally this reaction is supposed to be done during the day in direct sunlight. SWIM STRONGLY suggests to do so. If not in sunlight, go to Home Depot and purchase a small (like 150W or so) mercury vapour lamp, and keep it shining right on the flask when doing this. SWIM didn't take heed to that, so his yeilds were shit (like 30%). He didn't care much however, as what resulted from even such a low yeild was still a lot, plus things were kinda rushed, and SWIM just wanted to see if it could be done.

Anyways, reflux apparatus was setup using a rb two kneck (for SWIMS case, it was 1L, but size depends on size of rxn you plan on doing), and friedrichs condensor connected to the center kneck. At the top of the friedrichs, SWIM connected a straight vacuum adaptor (straight, like the kind used to adapt a funnel for vac. filtration, not the curved kind used for distillation), with a glass stopper closing it off, and a hose from the barb running out of a window for fume control.

A funnel was fitted on the side kneck, and some boiling stones were added, then the toluene was poured in. SWIM used a couple hundred mL's, but like SWIM said, it doesn't matter really how much you make, so amounts are up to you.

Now let me desrcibe how the gas generator SHOULD be built. SWIM says should because like a dumbass SWIM was in a rush and wasn't thinking and didn't do a good job building a gas generator. That resulted in major chlorine leaks, probably some lung damage, and frequent evacuation of the lab, which wasn't fun.

Anyways, another two kneck rb should be fitted with pressure equalized addition funnel, and the second kneck should be fitted with some rubber tubing. The tubing should run all the way through the second kneck of the main apparatus (after you remove the funnel of course) down to the bottom of the toluene. Charge the gassing apparatus with HCl acid, and the add. funnel with bleach. bleach is dripped into the HCl acid to create chlorine gas.

The procedure is done by heating the toluene to a reflux. Then start gas generation, to bubble the chlorine through.

SWIM had gassed with an ass of chlorine. SWIM had gassed multiple times. As in gassed once but didn't last long and pressure in gassing aparatus would wane.

The toluene would start to creep up the gassing tube, so SWIM would releive the pressure, empty the gassing apparatus and recharge it. SWIM did this like three times. However, if you design your apparatus properly and use enough bleach and HCl, you shouldn't have to much of a problem.

After wards the shit was simply cooled, and the apparatus was dismantled and cleaned.

All in all it took about four hours, which can be done quicker if you take heed to the things I said I should have done.

Now, I do not know the soluability of chlorine in toluene, but afterwards the shit reeked of chlorine. SWIM had to stop for the moment, so the flask was stoppered and set aside overnight.

The next day upon observation of the flask, SWIM had noticed a white whispy fog in the flask that looked kinda familiar. When SWIM removed one of the stoppers and blew into the flask, some of this fog came out. It looked like HCl fog that you see sometimes in the separatory funnel when you are titrating some freebase or something. SWIM wafted some toward his nose, and the smell plus the stinging definitely said it was HCl gas. "Good", SWIM thought. "That means that some benzyl chloride was formed".

1PhCH2 + 1Cl2---->1PhCHCl + 1HCl

The HCl is not readily soluable in boiling toluene, so it is driven off as it's formed, effectively keeping the equilibrium shifted in favour of benzyl chloride.

The equation for the gas is:

1NaOCl + 2HCl---->1NaCl + 1H2O + 1Cl2

The boiling stones and benzyl chloride/toluene solution SWIM had left over in the flask was left in the flask, as it was used as is for producing benzyl cyanide.

Thats it!! If better lighting was used, or a LiOCl method, then it's quite easy to produce asses of benzyl chloride. It's pretty cool when you can synthesize a major drug precursor from toluene and HCl acid from the hardware store, and bleach from the grocery.

Running out of time for now, so next up is preparation of cyanide and conversion of the benzyl chloride to benzyl cyanide.

Was wondering just last night an:"wtf is Mad man?! He never updated his P2P diaries and I hope he's alright!" <A HREF="http://users.pandora.be/eforum/emoticons4u/crazy/245.gif">http://users.pandora.be/eforum/emoticons4u/crazy/245.gif" width="90" height="90 (http://users.pandora.be/eforum/emoticons4u/crazy/245.gif" width="90" height="90)</A>



Good to see you're back man.



Jam.

Right on Mad! Glad you didn't wake up dead. Keep on keepin' on!

Why make p2p?

Wouldn't it be more pleasing to do a wacker on safrole to get mdp2p?

Your doing alot of work just to end up with racemic amph when you could be making mdma.

Step two:

Benzyl Cyanide From the Chloride

Next, SWIM simply refluxed a solution of mixed cyanide salts (NaCN/KCN) in H2O with the benzyl chloride solution from the first step. Once again, due to severe lack of funding (man we were broke as fuck, didn't even get to have any weed for that whole week either!), and well, to the fact that the only alcohol we had in the entire fucking house was half a bottle of vodka. Which got drank the night before anyway.

So no alcohol was used in this procedure, although once again SWIM would suggest to use it. Like SWIM had said about shortcuts he took in making the benzyl chloride,

my yeilds were low. It was done haphazardly, with tons of shortcuts, impure precursors (toluene/benzyl chloride, didn't bother to distill the chloride), but it still

worked. Plus SWIM din't care, he had tons of time, but no money. So I had to make do with what was on hand (plus no running water for half the week cause the well pump broke but thats another story).

The apparatus used was pretty much the same setup used for benzyl chloride, with the gas generator removed. In fact, one could make the chloride, remove the gassing part, add funnel and add ingredients for making the cyanide,and replace with a glass stopper (by the way all glassware has 24/40 tapered ground glass joints).

You still need a tubing going out the window for fume control plus incase any HCN evolution while doing this. For those living somewhere where you think there might be

someone to smell the fumes or see the a rubber hose sticking out of ones window, run it into a gas trap containing NaOH solution to neutralize any HCN that may evolve (same with the synthesis of the chloride, as any

Cl2 that gets through is converted to NaOCl, and HCl to NaCl). SWIM was in the woods basically and it was done at night so he just poked a hole in the screen and

shoved the exhuast tubing several feet out of the window. Old t-shirts were packed around the tube and across the bottom of the window, so when it was shut it created a

kind of seal, instead of having the window cracked some.

Now in the procedure at rhodiums, they used 10 parts cyanide salts, and 8 parts benzyl chloride. They dissolved the cyanide in 450mL water. Well, when SWIM had made

his benzyl chloride he had weighed the toluene before hand and wieghed it again afterwards, figuring his yeild was around 25%-30% of the chloride. SWIM used

that to figure out how much cyanide to use. From that you can figure the amount of water to use. If SWIM recalls correctly, SWIM thinks it ended up being around 40g of KCN used (although SWIM really had unkown mix of

NaCN/KCN, mostly KCN, more on that later).

Let me see, that means since it goes like this:

1KCN + 1PhCHCl----&gt;1PhCHCN + 1KCl

That would mean SWIM had about 77g of the chloride. So make sure you weigh your toluene before, then make your benzyl chloride and weight it again to figure out the amount of benzyl chloride you have (if you don't distill it), which you'll use to

figure out how much cyanide you need. With 40g cyanide SWIM used about 36mL of H2O, which was added first. Then the crushed cyanide was added (it was still pretty

chunky).

SWIM then replaced the funnel on the side kneck with a stopper. The mixture was heated until reflux ensued. This was held for 4 hours. The solution stayed a

greyish color for the whole time, and became brownish over time (on top of the grey).

Afterwards it was cooled back to room temp. Everything was dismantled and cleaned very well. The rb flask used

to reflux the mixture was washed several times, but there was still a greyish residue on the flask. SWIM had to add some fresh boiling stones and some soapy water

and swirl the hell out of it to kinda scrape the residue off (which worked well) so the flask would be clean.

The reaction mixture was poured through a filter fitted to a 1L separatory funnel, and the aqueous was separated from the organics. Dispose of the aqueous layer properly as it may still contain some cyanide.

SWIM then poured into appropriate sized rb flask and and connected that to a distilling column. That was connected to three-way distilling adaptor, which was fitted

with liebig condensor on the angled part. The top was fitted with thermometer adaptor and thermometer with -10C

to 350C range, and nescessary length of immersion. At the receiving end, an angled distilling adaptor was added (it was actually a vacuum adaptor, which was fitted with the exhuast hose for fume control), which led to an erlenmeyer that was used to collect forerun. Another erlenmeyer was used to collect the cyanide. Again all

joints were 24/40 in size.

Organics were then distilled. The benzyl cyanide collected was clear and had no color. It smelled like dirt. Like a soil smell I mean, maybe even with a hint

of ammonia. It probably could have used another distillation, so keep that in mind.

The Cyanide

The cyanide salts used in this were actually made before the benzyl chloride was even made. Let me first say that cyanide is dangerous as hell. I mean really dangerous. SWIM looked up all MSDS data he could find before attempting any of this. He didn't have any poppers, but two big ass bottles os thiosulphate were on hand in case of cyanide poisoning. It can be very easy

to accidentally ingest cyanide, as it takes very little to kill a person. 1KG of cyanide salts is enough to kill something like 20,000 people, as it can take as little

as 50mg to kill. PLEASE BE CAREFUL IF ATTEMPTING THIS PROCEDURE. Also SWIM is not responsible for anything anyone who reads this does or tries to do, as SWIM

reminds it's illegal to make drugs in most countries.

The fact SWIM was working with cyanides made him paraniod as hell whenever using them. Gloves were worn at times. Proper ventilation of used. Every peice of glassware used for something with cyanide in it was washed asap with hot soapy water. SWIM would wash the gloves, take them off, then vigorously wash hand immediately

after handling anything related to cyanide. Plus whatever sink that was used for all this was washed good afterwards.

Now SWIM went and got an extension cord, and hooked up the heating mantle outside. This has to be done outside due to any evolution of HCN. In a rb flask SWIM had

mixed 8 parts potassium ferricyanide and 3 parts sodium carbonate. The ferricyanide was weighed and added to the flask first. Then the carbonate was added. SWIM

shook the flask all kinds of ways to mix the two powders. Then it was placed in the heating mantle and the mantle

was turned on full blast.

For a while, nothing really happened. Then the mixture started to turn darker and darker. Once it had started to get nice and hot, SWIM caught a whiff or two of cyanide just standing there, so it was left by itself

while SWIM went back inside. Now SWIM has never smelled any form of cyanide before, but he has heard it smells like burning almonds. Well, when he did this and then

all of a sudden smelled a sweet smell, that was exactly like some damn almonds, SWIM new what it was, and hoped to god it wasn't a lethal dose he just smelled (it wasn't enough to have any effect, did I mention I was paraniod?).

After about an hour SWIM took some deep breathes and held the last one, and ran back outside to check on it. The mixture is supposed to turn liquidy and bubble, but

it had done nothing but turn a dark ass blackish grey color. But it didn't really look liquidy. So SWIM though he would let it sit another 30 minutes and check

on it.

When he did, it was finally liquidy, and bubbling quite a bit. So it was left for another 30 minutes or so. When SWIM came back, the flask contained a blackish solid

mass that looked gooey and had stopped bubbling. The procedure had said to decant the liquid material from the solid material, but SWIM couldn't tell what was fluid and what was solid. SWIM also did this outside

in the dark, so it was hard to really see the flask.

Upon disturbing the flask however, the shit started moving and turned out to be fluidy anyway.

So SWIM went ahead and got a big plate. The flask was removed, and SWIM started to decant. Low and behold the fluid that came out of the flask was not black, but

more greyish white (the ferricyanide is reddish orange and the carbonate white). Once most of it was poured off, there were some solids in the flask noticed. SWIM

was able to decant most of the molten cyanide before the dark stuff and solids started to come out.

Within minutes the shit poured on the plate began to crackle and pop as it solidified. Now SWIM suggests to

place the flask back in the mantle (after it's cut off of course) and allow to cool. SWIM made the mistake of setting the flask down outside not thinking after pouring the molten cyanide. SWIM was on the side of a

mountain, plus it's winter, so it was very cold outside. Plus it was drizzling, so the ground was wet and cold. When SWIM came back to the flask for clean-up, SWIM

had discovered it had spiderwebbed, so it was wrapped in several plastic bags and thrown in the lab trash. Good thing for SWIM it was one of the older flasks, and

not one of the newer ones, or else SWIM would have been pissed.

Anyways, the solid left on the plate was broken up and the chunks were placed into a freezer bag. This was quadruple bagged, and smashed up with a hammer. It was still pretty damn chunky, but it was crushed enough to fit through the kneck of the funnel so it was used as is. It was greyish white in color.

Now the ferricyanide SWIM had used was lab grade, and the carbonate was from a bottle of sodium carbonate pH adjuster for pools. However, if one does not want to, or have the resources to purchase a bottle of

ferricyanide, it possible to make your own from scratch.

According to the procedure at Rhodiums, rust, charcoal, and sodium carbonate are mixed together and heated. The ingredients react together with nitrogen in the air

(our atmosphere is comprised mostly of nitrogen), producing the ferricyanide. It's then cooled, and chipped into some hot boiling water, which is filtered.

Evaporate to yeild the ferricyanide. SWIM has never done this though so he doesn't know how good it works, or how it runs. So

caveat emptor I guess.

Well, that was a long one. Coming up next is hydrolysis

of the benzyl cyanide with sulfuric acid, giving

phenylacetic acid.

Why do all that typeing lengthy writeups when you could just do this?

http://www.worldwideschool.org/library/books/sci/chemistry/OrganicSynthesis/chap3.html

straight to the pointƒ

http://www.worldwideschool.org/library/books/sci/chemistry/OrganicSynthesis/chap17.htmlƒ

quote:

Why make p2p?



Cause I like meth. All the time, energy, and money SWIM has spent scraping matches and buying and cleaning pills and blah blah blah to get inconsistant results everytime could be spent on making P2P instead. The same amount of time, effort, and money SWIM spends in two weeks doing small personal batches via HI/P could potentially make at least a pound of the shit via P2P. Plus it's the satisfaction when SWIM synthesizes something thats good, it pleases him. The satisfaction is much higher knowing SWIM made something entirely from scratch (like with the P2P, which ultimately was made with toluene and vinegar).

quote:

Wouldn't it be more pleasing to do a wacker on safrole to get mdp2p?



Nope, it would be equally as pleasing. SWIM isn't trying to dominate the market, and doesn't do MDMA all that often even if he were sitting atop a kilo of the shit. Besides, SWIM has an MDMA project thats been put off for a while due to several reasons, he's not gonna let a few kilo's of eugenol go to waste. And SWIM doesn't like to mess with palladium salts, too expensive. SWIM was thinking more of isomerization of the safrole, and nitration of the propenylbenzene, which will be reduced to MDA and some converted to MDP2P for MDMA.

quote:

Your doing alot of work just to end up with racemic amph when you could be making mdma.



So what? It's more than just about drugs. Chemistry is SWIMS passion, SWIMS life. It will be SWIMS career as well. Nothing in life is free, it either costs money or good old fasioned elbow grease (and no, not the elbow grease from accidentally putting your arm in some joint grease, goddamnit SWIM has a horrible knack for doing that).

What SWIM mean to say before he went off on a tangent, is that the same amount of time and work could be spent making a fucking face cream for all I care, I get more from it than a buzz.

quote:

Why do all that typeing lengthy writeups when you could just do this? http://www.worldwideschool.org/library/books/sci/chemistry/OrganicSynthesis/chap3.html

straight to the pointƒ http://www.worldwideschool.org/library/books/sci/chemistry/OrganicSynthesis/chap17.htmlƒ



Cause if anyone out there is like me, they can read shit from OS online and shit like that and be happy. However, it's easier to relate to someones personal experience, it gives people a sense of "hey, he did it, maybe it's not that hard afterall". Plus I had fun, it was a learning experience, and I don't mind typing it all up. You should go through my chemistry notebooks. There is nothing but pages and pages of write-ups, ideas, discoveries, speculations etc. I am good at writing chemistry papers, which will go good with my career goal as R&D chemist.

quote:Why make p2p?Right off the top of my head I got two reasons Bizzy.......#1-Lemon Drop <A HREF="http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif">http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif" width="90" height="90 (http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif" width="90" height="90)</A> .....#2-a gallon of P2P will yeild 30 pounds of dope.



quote:Your doing alot of work just to end up with racemic amph when you could be making mdmaThis comment is always only ever made from those that have never had the pleasure of doing a blast of P2P!!! On paper it may look inferior to ephedrine-based-meth, but in practice you will find many who will argue that they think the racemic-P-dope is better. Not dogging you here Bizzy....just pointing out the attributes and misconceptions of this Old-School Rxn.

Jam.

Swim doesn't know the chemistry behind it all, and doesn't care. Don't know if raceamidget meth is better than d-dick meth, or not, but remembers that prope dope was good stuff.

SWIMS opinion is that racemic dope is better. Most drugs are better in racemic form. We were talking of MDMA before, which is best used in racemic form.

quote:According to the procedure at Rhodiums, rust, charcoal, and sodium carbonate are mixed together and heated. The ingredients react together with nitrogen in the air

(our atmosphere is comprised mostly of nitrogen), producing the ferricyanide. It's then cooled, and chipped into some hot boiling water, which is filtered.

Evaporate to yeild the ferricyanide. SWIM has never done this though so he doesn't know how good it works, or how it runs. So

caveat emptor I guess.

That procedure on Rhodium is a piece of worthless shit. It's a close copy of a slightly better procedure from the Poor Man's James Bond, but the PMJB procedure sucks too. The guy who wrote up that procedure obviously never even tried it, otherwise he wouldn't have seen "purple" flames coming from a sodium compound.

If you want to make sodium or potassium ferrocyanide at home, you melt KOH or NaOH and stir blood meal into it. This is messy, tedious (lots of foaming, so close attentin is needed), and smells bad. If you want to make cyanides directly, see the info I've posted to the text files section here on TOTSE about making them starting with an alkali metal carbonate or hydroxide and urea or cyanuric acid. It's easy to do completely OTC and it scales up nicely.

P2P is some asskickin shit. SWIM remembers the days back when it was available far and wide. SWIM misses those days and that dope. RP/I2 dope is good but fuck man SWIM has to do it himself to get good shit. in the last couple years the ONLY dope SWIM has done he made himself. everything else sucks and is trash in SWIM`s experienced view. a buddy brought some over awhile back and SWIM looked at it and handed it back and said fuck you man SWIM aint doing that shit. dude says, it aint cut man i know for a fact. SWIM said so fuckin what it aint cut its trash out of the flask some fuckin cut might help it lol. SWIM said here try some of this. 20 min later he could well see SWIM`s point of view as well. he spent the next 9 hours with a box of old junky flashlights that had various broken and missing pieces and when all was said and done he had taken 12 flashlights and two good inkpens and made one little keychain flashlight that worked. SWIM just shook his head and told him he was a sketchin motherfucker lol.

d-l amph is better than d meth?

I doubt it

but wicked,

nothing beats a classic root

NeverSleepy

Exactly Right!

Why produce a product that is 50% from the start than one that is 100% active

And...

Whoever gets over 5 lbs out of a standard 4 litre jug (app gal) of phenlylacetone is merely adding a lot of cut as the 5 lbs is 'theoretical max yield anyway--we all know what that means

---

also, benzyl c. is difficult for those without the proper licenses

[This message has been edited by dan46 (edited 01-05-2004).]

Potassium Ferrocyanide = Case hardening powder, Used to harden med/high carbon steel.

The steel is heated to red hot (not spitting sparks) dipped into cyanide, cooled slowley, Heated up again, cooled slowly, the carbon comes outa the cyanide goes into the steel as a layer about 2mm deep, the second heating is to form a consistant change from the med carbon steel to the high carbon steel outside layer.

Also used to poison rodents. need s certificate to get it thou,

Get the amylnitrate First!

Wouldn't like to have to fuck around trying to drink thiosulphate.

Had to get some once before getting cyanide, the chemist instructed how to use it, then said by the time its sorted Swimmed be ded anyway. Get the asmylnitrate too!

And the hyacynth thing, is this p2p?

Swims got a old book about essential oils and it says p2p, or would this have changed by now?

The people who diss racemic dope are the ones who obviously have never tried it. You can sit there and speculate all day long about how the d is active and l isn't, so racemic since it contains l MUST be worse than pure d. Well whatever. To each his own I guess. Besides the racemate may just be less potent BY WEIGHT, but that doesn't mean jack shit to what the buzz is like. The buzz is much better from the racemate, smoother, and so much longer lasting. The kind of shit you here about where one line keeps you up for a couple days. Plus racemic dope is usually made by skilled chemists (because of the processes involved), so generally it's cleaner than you average rp/I2 you find on the street, plus it contains none of that unreduced ephedrine/iodoephedrine bullshit. I can't wait until the naysayers one day get to take a few breath-taking blasts from the pipe of some racemic product. I honestly beleive you'll change your mind. And people may say they have tried it, but how do you know where that dope came from? Because your dealer who was no doubt trying to sell his product told you so? Unless you sat down and watched somebody make the shit from phenylacetone, and then tried the product, don't go ranting and raving about phenylacetone dope.

By the way, SWIM has to let his girl use his vacuum cleaner (new apartment), plus has some obligations with a few friends later on, so the phenylacetic acid synthesis won't be posted until later tonight. Probably around 4 or so when SWIM is bored and tweaking. Besides there won't be anything to do or watch on TV, and SWIM is tired of seeing that same damn Girls Gone Wild infomercial over and over.

how about soneone who has knowledge of both including the p2p--push/pull---long wet reflux hi/i?

the hi/i slooow wet is fantastic if performed with care and properly washed at the end

i understand that much of the redp/i stuff is hastily performed p/p setups with poor washing at the end so what can you expect?

a properly done LONG 32 hour wet reflux with the red/i ingredients then proper washing

and cleanup kicks p2p even though i have a real love for the old days and the synth presented above

also, i suppose you could merely 'cut your 100% dextro to 'buffer' it to your liking

the truth is meth is meth...period

any other differences are due to impurities

and the L (levo) isomer is basically an impurity in a sense as it has no (none) effect whatsoever

if you find differences please do thorough cleaning of the end product and test again

--





[This message has been edited by dan46 (edited 01-07-2004).]

Wouldn't it be a bummer if your reductive amination fails, all that risky work, money invested and time down the poopshoot.

Sucessfully going from toluene to racemic dope has plenty of room for error in my opinion but swim hopes it turns out for ya cuz nothings worse than a failed rxn besides getting 25yrs in prison for a failed rxn.

I still dont see the benefit of this method compared to mdma production.

Why didn't you persue PPA instead? Much easier and more uses.

what spot on the planet does the mad chemist habitate

Sweet PPA? I love a sweet PP as much a the next man. But don't sweet PP belong in S&A?



Sorry! But, I been saying that since the FDA

banned it in cold remedies. I used to love

that stuff for nasal stuffiness. I've wanted

to whip some up just for my nose.

Pretty simple too, huh?

PPA?

Sweet PP Rules! Eh? (Say it to yourself a hundred times & you'll wunder about brain

damage too.) Maybe the FDA was right & it

does cause strokes & brain damage.

quote:Originally posted by Jamiroquai:

Why make p2p?Right off the top of my head I got two reasons Bizzy.......#1-Lemon Drop &lt;A HREF="http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif"&gt; <A HREF="http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif">http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif" width="90" height="90 (http://users.pandora.be/eforum/emoticons4u/fingers/fing32.gif" width="90" height="90)</A> &lt;/A&gt; .....#2-a gallon of P2P will yeild 30 pounds of dope.



quote:Your doing alot of work just to end up with racemic amph when you could be making mdmaThis comment is always only ever made from those that have never had the pleasure of doing a blast of P2P!!! On paper it may look inferior to ephedrine-based-meth, but in practice you will find many who will argue that they think the racemic-P-dope is better. Not dogging you here Bizzy....just pointing out the attributes and misconceptions of this Old-School Rxn.

Jam.



You took the words right out of my mouth This thread sure did bring back some good memories.I love lemon drop I love prope dope(p2p) Btw props to Madchem keep on keepin on.

Alright, the preparation of phenylacetic acid was a breeze. Until the workup.

It still wasn't that hard, but it should have went a little easier. Starting from

about 40g of the distilled benzyl cyanide (yeild was around 60% or so from

theory, of the cyanide from the chloride, from which around 77-80g or so was

used to make the cyanide). SWIM made 120mL of 70% sulfuric acid. Which

was 84g of H2SO4 dissolved in 36g of H2O, done very slowy and carefully

on the magnetic stirrer, in a beaker.

This was poured into erlenmeyer flask, and straight vacuum connector was

connected at the top. The top of that was stoppered. A hose was connected

to the vacuum connection and led out of a window. All joints were 24/40 of

course.

This was heated until it began to vigorously bubble, which heat was then

removed. It continued to bubble on it's own for quite a long time. At least an

hour or so. By then it pretty much stopped. Swirling the flask like mad made

it occasionally bubble more. The vacuum peice was disconnected, and

reconnected to the top of the friedrichs. The erlenmeyer was connected to

the bottom, and shit was heated again, until reflux.

SWIM had let it reflux an additional hour. The solution had gone a pale yellow

in color, but there still remained some organic layer on the top. It started out

as quite a bit on top, and began to shrink as the reaction proceeded (it was

the cyanide being consumed SWIM presumes). It had stopped really getting

smaller by the time that hour was up so SWIM removed from heat and poured

onto 200mL or so of crushed ice. It was left for like another 2 hours in which

the ice melted.

By then, SWIM had a pale yellow solution with a small organic layer still

on top, that smelled like a mixture between raw honeycomb and probably

piss. It wasn't really a nice smell, but then again it wasn't to bad, although

SWIM could see larger batches being pretty rank. There was no precipitate

like their should have been however.

What to do about this fucking organic layer. SWIM really wanted to avoid

another distillation right yet, so said fuck it and decided to just try to nuetralize

the whole mix with sodium carbonate (in retrospect, if it happens again SWIM

will just separate the organics and distill it), turning any remaining acid to it's

sulfate salt (which some precipitates), and turning all the phenylacetic acid

to a water soluable sodium salt.

This took an ass of time and carbonate to neutralize the mix. SWIM just kept

adding until it stopped bubbling. The mix was then filtered. It was poured

into the sep. funnel (1L), and the organics were separated. The piss yellow

solution was poured into a beaker. The solution was then boiled to about

half of it's volume to concentrate it, and acidified with H2SO4 until the damn

acid started forming a noticeable layer at the bottom of the water (finally), and

the solution was cooled. The phenylacetic acid solidifed and formed a greyish

white mass, that smelled like horrible honey/piss.

The acid was of course filtered out with coffee filters, and placed into another

beaker. Some water was heated up and SWIM spent the time waiting for it to

boil admiring the solid mass he had created. The boiling water was poured

onto the mass, filling the beaker up with around 400mL or so. It was stirred

vigorously at the same time with a pencil, breaking up the acid until everything

was homegenous. It was heated until it began to boil again, then it was decanted

through some more coffee filters. The filtrate was poured back into a beaker

and placed into the refriderator, overnight.

The next day SWIM had a beaker full of white kinda waxy looking pearlescent

material sitting at the bottom of a bunch of greyish-yellow water. It was decanted

and the phenylacetic acid spread out onto a plate, and allowed to dry.

Overall, SWIM got about an ounce of phenylacetic acid, which approximates to

about 60% yeild. SWIMS benzyl cyanide was no doubt still impure, plus next

time SWIM is going to let reflux longer, at least a few hours.

Not bad though, for taking an ass of shortcuts so far and using impure precursors.

Coming up next:catalysts and tube furnaces and P2P, oh my!

<A HREF="http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif">http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif" width="90" height="90 (http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif" width="90" height="90)</A>

Revisions and updates coming.

Sorry for my recent slackness!