I have been reading over this U4Euh synth, and was wondering what everyone thought of the procedure and the precursers.....

4-Methylaminorex Synthesis (Ice/U4Euh)


Information...

Ice is a norepinephrine potentiator (neuromodulator class). It has a characteristic look and feel, like white opaque ice, hence the name. Ice is currently a Schedule I drug as designated by the DEA (Drug Enforcement Agency) which means it is felt to have NO medical use whatsoever. It was originally researched for appetite suppressant ability, but never pursued, probably because it's too much fun. Ice is also synonymous with "U4Euh".

The document at Hyperreal.com describing the effects of Euphoria would be a good place to start. Anecdotally, it is said to help concentration and thinking - a sort of "make-you-smarter" drug, with a minor speed-like component to it. Time of action is around 4-6 hours (some say 14-16). Dosage varies but a good start is 20mg for a 150lb individual. It is smoked as the free base or the hydrochloride salt - both have relatively low melting points.


Reagents...
1.Phenylpropanolamine HCl (this needs to be prepared by you ahead of time)
2.Methanol
3.Cyanogen Bromide (this also needs to be prepared ahead of time)
4.Sodium Acetate
5.Sodium Carbonate
6.Water
7.Benzene (or similar)
8.Ether

Extraction of Phenylpropanolamine from OTC preparations

Extract Phenylpropanolamine HCl (PPA) from OTC diet pills by crushing and dissolving in 5mL ethanol and 5mL distilled water per gram of PPA. Decant solution onto the Buchner funnel and repeat with 2 more volumes of solvent. Use ethanol/water instead of just water because it has less tendency to form a colloid with any cellulosic binders present which would otherwise severely clog the filter paper.

Distill off most of the solvent then add cold water to dissolve all of the PPA solids. Basify to approximately pH 9 with 10% Sodium Carbonate or Sodium Hydroxide solution. Extract out PPA base using 3 volumes of ether of approximately 1/3 the volume of water. The ethanol will follow into the ether as well, but very little of the formed salt will.

Distill off ether/ethanol for later recovery of the solvents and weigh the amount of solid PPA base, mp 101C. The amount you process here determines, obviously, the amounts of everything else to use later on.

Forming the Oxazoline Ring
The ideal ratio of all the reagents is as follows...
1.0 Mole Phenylpropanolamine (MW: 151.2)
1.1 Moles Cyanogen Bromide (MW: 105.93)
3.0 Moles of Sodium Acetate (MW: 82.04)

The Sodium Acetate may be prepared by carefully adding an equinormal amount of Sodium Hydroxide to glacial Acetic Acid and drying theresultant salt at 120C for 15 minutes.

Here it is....

This compound should only be prepared in an area of *adequate* ventillation. A full covering fume hood is ideal (geez - make one, I did) or outside with the wind blowing away from you. Cyanogen Bromide acts on cytochrome oxidase just like any other cyanide and can kill you quite effectively and quickly. Also, it has been known to decompose spontaneously when impure.


1.Dissolve 15g (.142M) of Cyanogen Bromide in 50mL of Methanol at 0C.
2.Dissolve 19.5g (.129M) of Phenylpropanolamine and 31.8g (.387M) of Sodium Acetate in 300mL of Methanol at 0�C. Place this in a round bottom flask equipped with a stirrer magnet and addition funnel.
3.Add the Cyanogen Bromide solution to the flask though the addition funnel over a period of 15 minutes with stirring.
4.React for an additional 45 minutes at 0�C.
5.Evaporate solvents at reduced pressure and with gentle water bath heat (50C tops) - do not attempt to recover!
6.Dissolve the oily residue in water and then add saturated Sodium Carbonate solution until a white solid precipitates.
7.Filter this cake of white solid on the Buchner, then wash twice with ice cold water and dry in a vacuum dessicator.
8.Recrystallize the crude dried product from Benzene to yield ~63%.
9.*OPTIONAL* - Form the hydrochloride salt by bubbling HCl gas though the Benzene until white crystals fall out or shaking with 5% HCl and evaporating the water off.

This was taken from the Rhodium Archives. I will be putting up a synth for Cyanogen Bromide on Chemhead as soon as I find a good one. This synth was written by Eleusis.

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CHEMHEAD CHEMISTRY
http://www.angelfire.com/mi3/chemhead

Hmmm. I've looked at this in the past myself. But the only thing is cyanogen bromide is a bitch to make, and like it says, can kill you fast (I've read elusis/zwitterions synth, nasty shit, plus produces cyanide gas).

ok here is the only synth for Cyanogen Bromide that I have on my site. I believe that it came from Rhodium at some time or another. tell me what you think of it...
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Production of Cyanogen Bromide

Hey, in case you are still with us after trying out all my other fun-at-home projects, perhaps you feel ready to embrace *real* danger? How about making your own Cyanogen Bromide, which is about as fun-loving as a compound can get! You have immense toxicity in combination with that all-around party favorite - instability! Kids, *don't* try this at home.

This stuff is deadly toxic and unstable. It should only be prepared immediately before use (no storage whatsoever). Perform this reaction outside on a windy day, or with a good fume hood (no, I don't mean the fan over the stove). Cyanogen Bromide has been known to decompose explosively on standing... you have been warned.


Here it is...

For the first half of the reaction, assemble a ground glass joint setup consisting of a 500mL round bottom flask, a claisen adapter,an addition funnel in the sidearm of the adapter, and a thermometer down the center. Place this in an ice/water bath on a magnetic stirrer.

Add 50g of elemental Bromine to the flask, followed by 5mL of water and a stirrer magnet. Start stirrer, and reassemble the thermometeradapter such that the thermometer will read the liquid temperature. Dissolve 17g of Sodium Cyanide in 120mL of warm water and add this gradually to the flask through the addition funnel, taking care that the reaction temperature does not exceed 25-30C. The time it takesto add the NaCN solution is quite variable, but the total reaction time should be around 2 hours.

At the the end of this time, remove the claisen adapter and replace with a 3-way distilling adapter to which a 500mL round bottom flask is connected *directly* to the outlet tube. Insert the thermometer in conventional manner (to read the vapor temperature) and distill off the BrCN using a water or steam bath. It should boil at 60-62C.

Clean off all of the glassware, then add 10g of anhydrous Calcium Chloride to the receiver flask and reassemble the same setup aspreviously. Redistill the crude BrCN from the CaCl2 as before. Once all has been collected over the range of 60-62C, melt the solid inthe receiver by heating to 51C (note the closeness between melting and boiling!) and pour into a pre-weighed glass bottle. The yieldshould be 23-28g, or approximately 73-85% of the theoretical. If it will not be used immediately, it may be stored in the freezer, butshould be used as soon as possible


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CHEMHEAD CHEMISTRY
http://www.angelfire.com/mi3/chemhead

Uhh, definitly not something I would suggest to anyone to try. Can you post a link or a pic or something of the structure of methylaminorex? There has got to be another route somewhere. If there is a will there is a way right? I'll see if I can find anything out on chemfinder or something.

Besides, where are you gonna find a reasonable amount of NaCN? They dont just hand that shit out. Hmmmmmmmmmm.....

PPA is a prescription, not OTC. It comes most commonly in expectorants with guaifenisin.

4-Methylaminorex is virtually uncuttable and has a half life of over 8 hours. People complain it lasts too long(longer than methamphetamine in most cases)- fuck those people, they can't hang.

all right here is a link to the structure....
http://www.erowid.org/chemicals/4_methylaminorex/4_methylaminorex_chemistry.shtml

cyanogen bromide is contained in all the 4-methylaminorex synthesis that i've seen, and they are few and far between.

Yeah I know, but that doesnt mean there isnt another route. For instance, Shulgin uses LAH to reduce just about everyfucking thing in PIHKAL, which is impratical. But there are still other routes to most of he interesting compounds there.

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Thats just the way it is...
Things will never be the same..
Thats just the way it is.
I see no changes
All I see is racist faces
Misplaced hate brings disgrace to races.-2pac

AAAAAAA HAAAA! 4-methylaminorex synths are more common than you think slp. And guess what? I was reading through some posts at the hive earlier, and this post by rhodium is what I found. It gives procedures to make 4-dimethylaminorex from ephedrine and psuedoephedrine without cyanogen bromide, and will probably work equally as well for 4-methylaminorex from PPA.
Here is what Rhodium Posted:

quote:

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After reading J Chem Soc, 850-854 (1952), I found ideas for 4-Methylaminorex (4-MAR, U4EUh) syntheses, with or without the use of cyanogen bromide. All the examples below relates to the reaction of ephedrine and pseudoephedrine to form racemic 3,4-dimethylaminorex isomers, but the exactly same schemes should apply to phenylpropanolamine (PPA) to give 4-MAR. The two routes described are either the classic cyanogen bromide cyclization of PPA and formation of the carbamyl (substituted urea) derivative of PPA, followed by acid treatment.

Using the cyanogen bromide route, the cis-form of 4-methylaminorex can be had from the phenylpropanolamine isomer corresponding to pseudoephedrine (1S,2S)/(1R,2R) and the trans-form from the phenylpropanolamine corresponding to ephedrine (1R,2S)/(1S,2R). The cyanogen bromide procedures below aren't optimized, addition of 3 equivalents of sodium acetate and doubling the amount of cyanogen bromide would not produce a precipitation of ephedrine salts, thus making the procedure more effective (see other syntheses of 4-MAR on my site).

Using the "double racemic" phenylpropanolamine (1RS,2RS) would give equal amounts of racemic cis- and trans-4-methylaminorex. All the cis/trans isomers are active, as well as their respective stereoisomers. The trans(4S,5S) is the most potent, with an effective dose of 0.25 mg/kg (compared to dextroamphetamine considered active at 0.4 mg/kg and d-meth at 0.2 mg/kg). The cis isomers are of about 5 times lesser potency, but they are still pretty active, as they are about equipotent to racemic amphetamine, and with a 2-3 times longer duration.

Using the potassium cyanate route, it should be noted that only the PPA corresponding to the pseudoephedrine stereoconfiguration (1S,2S) or (1R,2R) can be transformed into trans-4-MAR (no cis-4-MAR is being produced either), the PPA corresponding to the ephedrine stereoconfiguration (1S,2R) or (1R,2S) will on the same treatment form trans-4-methyl-5-phenyl-oxazolid-2-one (which looks just like 4-MAR, but with a double bonded oxygen instead of the NH2 in the 2-position. It is an amide rather than an amine, so it should be removable using an acid-base extraction.

The byproduct amide trans-4-methyl-5-phenyl-oxazolid-2-one can be isolated and catalytically hydrogenated at room temperature in ethanol containing 5% triethylamine and 10 mol% Pd/C to form (S)-amphetamine in 90% yield, Ref: Chem Eur J, 3(8) 1370 (1997), but that is probably not particularly useful, but using the potassium cyanate scheme on substituted ephedrines (like the 3,4-methylenedioxy variety) would enable you to produce a stereoselective synthesis of (S)-MDMA, the more active isomer, together with the 3,4-methylenedioxy-trans-4-MAR for evaluation of its activity.


Experimental

N-carbamyl-(�)-pseudoephedrine

5g (�)-Pseudoephedrine hydrochloride (25 mmol) in 50ml methanol was added a solution of 2g potassium cyanate (KOCN, 25 mmol) in 150ml methanol, and the solution was heated under reflux for one hour. Potassium chloride was filtered off and the filtrate evaporated to dryness. The residue was recrystallized from 20ml of ethyl acetate to give 2.2g of the substituted urea as white plates, mp 140-141�C.

(�)-trans-3,4-Dimethylaminorex HCl

A solution of N-carbamyl-(�)-pseudoephedrine (1.65g, 75 mmol) in 24ml water and 15ml 2N HCl was refluxed for three hours, when the clear solution was cooled the (�)-trans-3,4-Dimethylaminorex hydrochloride precipitated. This was purified by basifying the solution, extracting it with benzene (can use any non-polar solvent here), and the solvent evaporated and the freebase converted to the hydrochloride by gassing with dry HCl in ether. Yield 1.9g, 84%, mp 225-229�C.

(�)-cis-3,4-Dimethylaminorex HCl (from (�)-ephedrine)

60ml of an etheral solution containing 3.5g (30 mmol) cyanogen bromide was added to 200ml of an etheral solution containing 11g (�)-ephedrine (66 mmol), whereupon 8.1g of ephedrine hydrobromide separated (50% based on ephedrine input, 33 mmol, mp 186-188�C) and was filtered off and washed with ether. The filtrate was concentrated to 25ml, and white needles (1.5g, mp 71-73�C) of (�)-cis-3,4-Dimethylaminorex freebase precipitated. The filtrate was concentrated further, and the residual oil treated with ethanolic hydrogen chloride. The product was recrystallized from a mixture of 25ml CHCl3, 10 ml acetone and 5ml ether yielding 4.2g of (�)-cis-3,4-Dimethylaminorex hydrochloride, mp 215-217�C.

(�)-trans-3,4-Dimethylaminorex HCl (from (�)-pseudoephedrine)

40 ml of an etheral solution of 1.75g cyanogen bromide (16.5 mmol) was added to a solution of 5.5g (�)-pseudoephedrine (33 mmol) in 100ml ether and 80ml benzene. In addition to precipitated pseudoephedrine hydrochloride (3.9g), (�)-cis-3,4-Dimethylaminorex hydrochloride (2.2g) was obtained upon treatment of the residual oil after evaporation of the solvent with ethanolic hydrogen chloride, mp 215-217�C, identical to the sample prepared above.

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Thats just the way it is...
Things will never be the same..
Thats just the way it is.
I see no changes
All I see is racist faces
Misplaced hate brings disgrace to races.-2pac

very nice find madchemist, seems like a much safer route than CNBr