University Of Technology Sydney-Centre for Forensic Science



Abstract:

The aims of this project were two fold. Firstly to further investigate the reaction mechanism of the reduction of N,N-dimethyl-3-phenyl-3hydroxypropylamjne via hydriodic acidl red phosphorus. Such a reaction is a cognate methamphetamine synthesis from ephedrine. The results of the investigation showed the reaction to be dependent on both light and temperature. Impurity formation was also studied in order to further understanding of the reaction mechanism. The reaction was monitored using gas chromatography/mass spectrometry (GC/MS) and nuclear magnetic resonance spectroscopy. (NMR)

The reaction was also subject to a quantitative analysis, which required preparation of the salts of the three main reaction components; the starting material N,N-dimethyl-3-phenyl-3bydrox;propylamine, the alkene intermediate N,Ndimethyl-3-phenyl-1-amino-2-propene. and the reaction product N,N-dimethyl-3-phenylpropylamine.

The second aim of the project was to investigate another cognate synthesis of methamphetamine also utilising N,N-dimethyl-3 -phenyl-3hydroxypropylamine. This reaction was a modified Birch reduction using lithium metal, anhydrous ammonia and saturated ammonium chloride. The reaction yielded the same product as the aforementioned HI/RP reduction. The mechanism involved was shown to be a one step reduction with no intermediates detected. Again GC/MS and NMR were used to monitor the reaction, however impurity profiling was unnecessary as no impurities were formed during the reaction. Such a result was very significant, as the modified Birch reduction may in the future replace HIIRP as the preferred route for the clandestine manufacture of methamphetamine from ephedrine/pseudoephedrine.



Note: This oddly enough in my book at least proves that the reduction in a birch is potentially free of impurities whereas HI/RP ain't.

Novel idea using ammonium chloride and look at the refrence to "modified birch in the future" seems to me that the birch may be in for an overhaul in its method discourse.

Jam.





[This message has been edited by Jamiroquai (edited 11-30-2003).]

hehe jam,now there is not going to be any ammonium chloride left in the world cause kirby is gonna buy it all,lol-----Green

Making or acquiring anhydrous ammonia has a major "pain in the ass factor", and even right now, is not very popular at all in the clandestined front. Basically, I honestly don't think it will ever replace HI reductions (no matter what the recyclant) in popularity at all.

If the birch could be done in other amine solvents (research still pending from other bee's who dare) that are easier to make/acquire/handle, then SWIM could see the birch definitely replacing many forms of reduction of pseudo and friends.

It's a shame too, as the birch is so fast, strong, clean, and simple. Yeilds if done properly are very high. Plus there is high (if not complete) conversion of pseudo to meth.

It seems to be a popular beleif by many that the birch dope they have tried has been shittier than properly HI reduced dope. SWIM can garuntee that this is true, but only because of an error on the chemist's part. The birch is such a strong reduction that it's typical to see some "cooks" take advantage of this by throwing in some pretty gakked up pseudo into the reduction (not to mention if the NH3 is not home-made or came from R717, then it has shit in it, but we won't go there). Yeah, the birch will cut through the gakks, but not without loosing some of it's power to the gakks first. Plus as the ever so popular saying goes, crap in=crap out.

Pure sparkly psuedo, clean NH3, and good clean Li that hasn't been exposed to much moisture/air in the proper amounts will create some great product.

Now with general knowledge of HI reduction mechanisms becoming more household tweaker knowledge, coupled with advances in producer/recyclant feild is making the HI reduction too easy. Especially when doing wet refluxes, as you have to be a complete newbee or blithering idiot to screw up.

More research needs to be and will be done on H3PO4--->H3PO3 conversion, which will narrow the HI reduction precursor list to only KI and H3PO4, and psuedo source of course. H3PO4 can be reacted with some KI producing 57% HI, purified by simple fractional distillation. The rest of the H3PO4 is converted to H3PO3. The recyclant, HI acid, and cleaned pseudo is combined and refluxed, producing meth.

The general skill of your average meth "cook" is increasing dramatically every month. Hell every day. SWIM remembers not to long ago how most street dope was $80 a gram brownish or tan shit, and the beloved shards were harder to come by if at all. Now, barely two years ahead, if SWIM were to purchase street meth, he would probably never see that brown shit again. All meth seen purchased by other people from streets recently has been nothing but shards.

As the cooks grow tired of the HI reduction, demand for HI reduction will go down. As the general skill level increases. This will also cause the demand for other reductions like the birch to also drop dramatically. Once these cooks (the goods ones, happens to all of them) get better and more skillfull more time and investment will go toward buying glassware and OTC chemicals required to prepare for simpler reduction methods.

SWIM personally would like to see (and probably will) the majority shell out the bucks (SWIMS saving up) for expensive (but still non-suspicious) hydrogenation catalysts

like Pd/C, which can be used over and over a bbunch of times before it becomes scrap. Think about it. If people have the time to pre-make 57% HI, and do 24 hour + reductions, then whats to stop them from making HI acid from H3PO4 and KI (all otc), and boiling pseudo in enough HI acid for a few hours, (maybe with a little Zn metal thrown in to produce ZnI2 lewis acid catalyst even) supporting high conversions of pseudo to iodoephedrine. One could then dilute the solution with H2O, and boil off any remaining acid, followed by concentration of rxn fluid, and finally evaporation to yeild an easily reduce-able intermediate.

Formic acid can be made a plethora of otc ways, which can be reacted with otc aqueous ammonia solutions producing ammonium formate (NH4COOH). Of course a day or two could be spent easily producing copious amounts of both 57%HI and NH4COOH.

From there, acetic acid, the iodo-ester (or ester of choice), Pd/C can be combined, and refluxed with NH4COOH for an hour or so. Viola, high yeilds of optically pure methamphetamine. WOrk-up is no harder than any other work-up for any other reduction (birch, HI and the like).

That is just one idea thrown out there for the future reductions of yore. Advances in catalysts are happening to, and more research needs to be done on a catalyst like the still experimental nickel oxide on charcoal Pd/C alternative. Maybe advances in the electrolytic feild will take place and our children will be zapping solutions with electricity to make their meth. Or OTC P2P production will take over when pseudo finally gets banned one day. Or advances in akabori methods opening up way to very cheap and otc PPA/pseudo production. You never know with as smart as the "underground clandestined elite" is getting nowadays.

SWIM still thinks the HI reduction will remain the most popular for a very long time however, as like said before it's so simple and easy to do. All it takes is time, and HI methods can produce some of the highest quality cleanest dope around.

Back in the day SWIM used to see birch reductions quite frequently on the boards, but besides the general newbee birch questions, the amount of people actually using this reduction has been noticed to have dropped dramatically. The birch is dying!

Well, good write up. I think that you are correct, however the I is going to be banned rather than psuedo. The companies doing manufactor of cold pills have very deep pockets. And money talks.

I am interested in Pd that you speak of, however. You combine it with I? Or RP? I will read again. Again, props on the reaserch.

Follylover:

I am in a rush right now, will get back to you.



I just wanted to quickly say upon further research heating H3PO4 to 200C to try to obtain H3PO3 is a useless death-trap. Even if H3PO3 does get produced, it'll readily get oxidised by the air back to H3PO4. Plus H3PO3 decomposes at 180C to deadly phosphine!

The true source lies within fertilizers. Foliar solutions containing "phosphite" or "phosphonate" (PO3 3-) salts and a couple other easy to remove knick-nacks are widely available cheap and otc. Add 3H+'s to that PO3 3- ion, and voila H3PO3. So otc and easy SWIM shat himself. Write-ups abroad!

Well I know where to get H3PO3 flakes and if I can so can you guys.

But if you PM me Mad at the new site I'm sure I can oblige in passing you a key.



Jam.

quote:Originally posted by madchemist:

Making or acquiring anhydrous ammonia has a major "pain in the ass factor", and even right now, is not very popular at all in the clandestined front. Basically, I honestly don't think it will ever replace HI reductions (no matter what the recyclant) in popularity at all.

If the birch could be done in other amine solvents (research still pending from other bee's who dare) that are easier to make/acquire/handle, then SWIM could see the birch definitely replacing many forms of reduction of pseudo and friends.

It's a shame too, as the birch is so fast, strong, clean, and simple. Yeilds if done properly are very high. Plus there is high (if not complete) conversion of pseudo to meth.

It seems to be a popular beleif by many that the birch dope they have tried has been shittier than properly HI reduced dope. SWIM can garuntee that this is true, but only because of an error on the chemist's part. The birch is such a strong reduction that it's typical to see some "cooks" take advantage of this by throwing in some pretty gakked up pseudo into the reduction (not to mention if the NH3 is not home-made or came from R717, then it has shit in it, but we won't go there). Yeah, the birch will cut through the gakks, but not without loosing some of it's power to the gakks first. Plus as the ever so popular saying goes, crap in=crap out.

Pure sparkly psuedo, clean NH3, and good clean Li that hasn't been exposed to much moisture/air in the proper amounts will create some great product.

Now with general knowledge of HI reduction mechanisms becoming more household tweaker knowledge, coupled with advances in producer/recyclant feild is making the HI reduction too easy. Especially when doing wet refluxes, as you have to be a complete newbee or blithering idiot to screw up.

More research needs to be and will be done on H3PO4--->H3PO3 conversion, which will narrow the HI reduction precursor list to only KI and H3PO4, and psuedo source of course. H3PO4 can be reacted with some KI producing 57% HI, purified by simple fractional distillation. The rest of the H3PO4 is converted to H3PO3. The recyclant, HI acid, and cleaned pseudo is combined and refluxed, producing meth.

The general skill of your average meth "cook" is increasing dramatically every month. Hell every day. SWIM remembers not to long ago how most street dope was $80 a gram brownish or tan shit, and the beloved shards were harder to come by if at all. Now, barely two years ahead, if SWIM were to purchase street meth, he would probably never see that brown shit again. All meth seen purchased by other people from streets recently has been nothing but shards.

As the cooks grow tired of the HI reduction, demand for HI reduction will go down. As the general skill level increases. This will also cause the demand for other reductions like the birch to also drop dramatically. Once these cooks (the goods ones, happens to all of them) get better and more skillfull more time and investment will go toward buying glassware and OTC chemicals required to prepare for simpler reduction methods.

SWIM personally would like to see (and probably will) the majority shell out the bucks (SWIMS saving up) for expensive (but still non-suspicious) hydrogenation catalysts

like Pd/C, which can be used over and over a bbunch of times before it becomes scrap. Think about it. If people have the time to pre-make 57% HI, and do 24 hour + reductions, then whats to stop them from making HI acid from H3PO4 and KI (all otc), and boiling pseudo in enough HI acid for a few hours, (maybe with a little Zn metal thrown in to produce ZnI2 lewis acid catalyst even) supporting high conversions of pseudo to iodoephedrine. One could then dilute the solution with H2O, and boil off any remaining acid, followed by concentration of rxn fluid, and finally evaporation to yeild an easily reduce-able intermediate.

Formic acid can be made a plethora of otc ways, which can be reacted with otc aqueous ammonia solutions producing ammonium formate (NH4COOH). Of course a day or two could be spent easily producing copious amounts of both 57%HI and NH4COOH.

From there, acetic acid, the iodo-ester (or ester of choice), Pd/C can be combined, and refluxed with NH4COOH for an hour or so. Viola, high yeilds of optically pure methamphetamine. WOrk-up is no harder than any other work-up for any other reduction (birch, HI and the like).

That is just one idea thrown out there for the future reductions of yore. Advances in catalysts are happening to, and more research needs to be done on a catalyst like the still experimental nickel oxide on charcoal Pd/C alternative. Maybe advances in the electrolytic feild will take place and our children will be zapping solutions with electricity to make their meth. Or OTC P2P production will take over when pseudo finally gets banned one day. Or advances in akabori methods opening up way to very cheap and otc PPA/pseudo production. You never know with as smart as the "underground clandestined elite" is getting nowadays.

SWIM still thinks the HI reduction will remain the most popular for a very long time however, as like said before it's so simple and easy to do. All it takes is time, and HI methods can produce some of the highest quality cleanest dope around.

Back in the day SWIM used to see birch reductions quite frequently on the boards, but besides the general newbee birch questions, the amount of people actually using this reduction has been noticed to have dropped dramatically. The birch is dying!

Chem this was a super read and i agree with most of what you said.the part of it about the popularity of reductions differs as with were you are!Swim lives in a big city but surrounding that there aint nothin but cornfields for a four state radius so you can imagine annie is the prefered reduction.Its kinda funny cuz birchin is easy but if you dont really no what your doin your right you get sue dough and a little bit of meth.Swim has seen plenty of toothless nonreducin birchers in his day.Hes also found out aint no since helpin em cuz either they dont understand or they just love there sue dough.But anyway around here annie is a big thing.Keep up the good reads!TMG

jam,

did you get my question in the thread

the great kirby

I guess I didn't man.

What's up?



Jam.

Pd/c only works with chloroephedrine.

Are you guys forgeting about the cyanate rout to aminorex analogs?

You can easily make sodium cyanate by heating baking soda, urea and a little water, then use it to turn your pseudo/ephedrine into aminorex.

100% OTC ICE

Oh?!

Why don't you go take that 100% OTC ICE of yours and shove it straight-up your ass cock-bite?!

You still ain't welcome here and ain't nothing changed but the date since you last surfaced so go back to the Hive and go talk about your analogs and what you SAY they producewith Kats who care.

I mean nobody and I mean nobody at totse(which is a pathetic position to be in since this IS TOTSE) likes you dude.



Comprende' Puto?!



Jam.

Geeze, take it easy on him, Jam! The poor fuck probably has ChickenSutt Syndrome, or maybe Sutt's up his ass. Or maybe he's the chicken up Sutt's ass? Ah! The possibilities are endless!

quote:Originally posted by kman:

Geeze, take it easy on him, Jam! The poor fuck probably has ChickenSutt Syndrome, or maybe Sutt's up his ass. Or maybe he's the chicken up Sutt's ass? Ah! The possibilities are endless!

LOL

im with jam all the way on this one