Totse.com is no longer available!
This is a static archive of what the website used to be.
Check out the new articles and visit the community at Zoklet.net

Log in

View Full Version : Amphetamine from Phenylalanine


blacklung
2008-06-21, 07:13
I just got done reading Fester's new 2nd Edition (its less than a month old) of Advanced Techniques. His phenylalanine section is great.

Check it out:

D,L-Phenylalanine from L-Phenylalanine:
US Patent 3,213,106

Ethyl or Methyl Ester of Phenylalanine from D,L-Phenylalanine:
US Patent 5,744,611

Phenylalinol from the Ester of Phenylalanine:
Chem. Abstracts, Vol. 15, page 1289
US Patent 5,744,611

Sodium Bromide + Phenylalinol to get the bromo derivative, general procedure (search for making n-butyl bromide)

Phenylalinol bromo derivative --> Amphetamine
J. Org. Chem Vol. 16 pages 1731-35

Methylate Amphetamine --> MA
Tet. Lett. Vol. 48 pages 7680-82 (2007)

Problems:
Uses sodium borohydride, hard to find.
Uses palladium

Still neato, though.

stateofhack
2008-06-21, 09:06
I just got done reading Fester's new 2nd Edition (its less than a month old) of Advanced Techniques. His phenylalanine section is great.

Check it out:

D,L-Phenylalanine from L-Phenylalanine:
US Patent 3,213,106

Ethyl or Methyl Ester of Phenylalanine from D,L-Phenylalanine:
US Patent 5,744,611

Phenylalinol from the Ester of Phenylalanine:
Chem. Abstracts, Vol. 15, page 1289
US Patent 5,744,611

Sodium Bromide + Phenylalinol to get the bromo derivative, general procedure (search for making n-butyl bromide)

Phenylalinol bromo derivative --> Amphetamine
J. Org. Chem Vol. 16 pages 1731-35

Methylate Amphetamine --> MA
Tet. Lett. Vol. 48 pages 7680-82 (2007)

Problems:
Uses sodium borohydride, hard to find.
Uses palladium

Still neato, though.

Good stuff but:

sodium borohydride= electric car fuel cell! Look online and you will know what i am talking about!
Palladium= photochem stupplier:)

There is a big big thread about this on WD! Check it out:)

stupid noob
2008-06-21, 16:18
Good stuff but:

sodium borohydride= electric car fuel cell! Look online and you will know what i am talking about!
Palladium= photochem stupplier:)

There is a big big thread about this on WD! Check it out:)
Also, mufflers.

fcknut
2008-06-21, 17:19
Also, Aldrich ;)

stateofhack
2008-06-21, 18:34
Also, mufflers.

For palladium?

Also, Aldrich ;)

i c wut u did thar...oh wait your being serious ? :(

stupid noob
2008-06-21, 18:40
For palladium?



i c wut u did thar...oh wait your being serious ? :(
I should have been more specific. I meant the exhaust system in general. The catalytic converter contains a Pd metal catalyst. Either Pd or Pt, I forget. Maybe a combination?


I know a lot of crackheads around here steal them and sell the metal catalyst.

blacklung
2008-06-21, 19:09
Yeah I was about to say, Catalytic converters.

The ref calls for either Pd, or Pt; either one will work.

One could also use Zinc, but yields are 10% or so. With the former, yields are from 80 to 90%.

stupid noob
2008-06-21, 21:56
Yeah I was about to say, Catalytic converters.

The ref calls for either Pd, or Pt; either one will work.

One could also use Zinc, but yields are 10% or so. With the former, yields are from 80 to 90%.
I would say that would make it worth the hefty price tag.

stateofhack
2008-06-22, 01:12
I should have been more specific. I meant the exhaust system in general. The catalytic converter contains a Pd metal catalyst. Either Pd or Pt, I forget. Maybe a combination?


I know a lot of crackheads around here steal them and sell the metal catalyst.

haha crackheads selling catalyst! new one to me! Am i correct to say that a "used" exhaust will not to as well? I know the catalyst do not get used up and what not, but we have to remember they probably get poisoned.... reducing there efficiency!

i get my hydrogenation catalyst from photo chem supplies, seriously worth it! Not as cheap, but the prices are still pretty darn good and the quality is top!

stupid noob
2008-06-22, 02:39
I don't think it would be much of a task to clean it up.

nshanin
2008-06-22, 20:13
I do believe JP had a Phenylalanine-->Meth post; let me see if I can get it from memory:

1. Strecker degradation of L-PA to phenylacetaldehyde (just throw some bleach on it, or pure NaClO if you have it). This process is far more useful than the pedo lets on, I'm sure you could do many fun rxns with the byproduct of ClO- and several 3,4 dioxide derivatives of various Phenethylamino acids. And tryptophan too!(just look at the structure, you'll see what I mean)

2. Oxidation to phenylacetic acid--JP recommended diammine silver, but I found a cheaper, more versatile, and OTC oxidizer through an ACS article (had to go to uni to look it up for free :mad:): http://www.mediafire.com/?uzydgqyi0zz Here you would react your acid (as well as some vinegar) with some calcium compound for the next step; depending on the Ka of PhAc acid, you might be able to get away with throwing some CaCO3 into it, but I have yet to look that up. Calcium hydroxide sounds easier anyway.

3. Dry distillation of Calcium Phenylacetate with Calcium acetate to yield P2P--this is the difficult step; as dry distillation isn't particularly OTC, and if you used the diammine silver you could easily make an explosive silver compound (and not the fun kind). I've searched quite a while for an effective way to dry distill this, and unless you want to use lead acetate (suspicious, expensive, leaves a massive chunk of lead in your glassware), you'll need ridiculously high temperatures that are out of the grasp of many (though JP did say that it could be done at 180 celsius, I had difficulty believing him after reading several meth cooks' experiences with Ca(Ac)2). Somewhere around here you should purify your ketone; I believe Rhodium has a good (and quite OTC) description of how to do this with bisulfite.

4. Afterwards, you're supposed to know how to get the methylamine to reductively aminate the P2P, but I have several testimonials of people that say that simple glycine, when heated, will decarboxylate to methylamine. If this is true, the only semi-difficult (or semi-expensive, semi-illicit, etc.) item to attain will be your dry distillation tube, which most clandestine chemists have in the form of a Liebig condenser anyway.

And no dicking around with expensive catalysts, NiCl2 is cheaper than piss. :)

FullMetalJacket
2008-06-23, 04:31
Who needs glycine for methylamine when hexamine can be bought by the kilo?

nshanin
2008-06-23, 05:47
Who needs glycine for methylamine when hexamine can be bought by the kilo?

Meh, just throwing it out there.

fishtea
2008-06-24, 03:27
Can all catalysts be reused indefinitely as long as you can extract it back out of the end product?

stupid noob
2008-06-24, 05:45
Can all catalysts be reused indefinitely as long as you can extract it back out of the end product?
I think there are a few reactions where some of a catalyst is "used up", but for the most part, you are correct, if it can be reclaimed and cleaned of impurities, it can be used again.

Von Bass
2008-06-24, 15:42
As far as I know, by definition a catalyst merely shoves the reactants via different mechanistic pathway*, without being structurally, chemically, whatever the hell, altered in the reaction.

But in quite a few complex reactions, recovery of the catalyst is so difficult that its not worth while. I would also imagine in something requiring a two step reaction, say first unspecific catalytic hydrogenation and then oxidation, the metal catalyst (nickel for example) could be oxidised in the next step.

*I know that was a big generalisation. :)

fishtea
2008-06-24, 16:22
Really? I read somewhere that catalysts pull at the atoms of certain compounds putting more space in between each atom, making the atomic bonds weaker hence more susceptible to attack. I haven't got into the details of catalysts yet but its an interesting subject.

Pooter
2008-06-24, 19:09
They work by decreasing the bond dissociation energy required for each mechanism.

Basically, a catalyst is a conductive metal that can hold onto spare e-'s while things react. Just redox. They actually do react, and in some intermediate steps they are unrecognizable(as catalysts), but they are always regenerated back.
I should have been more specific. I meant the exhaust system in general. The catalytic converter contains a Pd metal catalyst. Either Pd or Pt, I forget. Maybe a combination?


I know a lot of crackheads around here steal them and sell the metal catalyst.
lol, I've bought pd from crackheads for dirt cheap. This one fool named Chicago sold to me and he was all hustling me with his "Young boy, you wanna buy some this shiny platiunum. Give it to a bitch get you some big o ass in seconds". It was so cheap, but I was a bit disappointed that it wasn't pure platinum(lol dumb bitch).

Von Bass
2008-06-24, 19:26
They work by decreasing the bond dissociation energy required for each mechanism.

Basically, a catalyst is a conductive metal that can hold onto spare e-'s while things react. Just redox. They actually do react, and in some intermediate steps they are unrecognizable(as catalysts), but they are always regenerated back.

Fair enough, I assume my teachers weren't quite telling me the whole truth, although we haven't completely covered catalysts yet, thanks for explaining that. I assume you're not also taking enzymes into that definition, I know the active site / lock and key theory to be roughly correct at least.

Pooter
2008-06-25, 21:20
Fair enough, I assume my teachers weren't quite telling me the whole truth, although we haven't completely covered catalysts yet, thanks for explaining that. I assume you're not also taking enzymes into that definition, I know the active site / lock and key theory to be roughly correct at least.

Yeah, the difference between an enzyme and catalysts are that platinum is one molecule, and say RNA transcriptase is a fucking giant protein with hundreds of complex peptides.

What's crazier is that some vital enzymes also require cofactors(enzyme catalysts) to catalyze their own catalyst reactions.

hydroponichronic
2008-08-08, 21:44
Wow, so this thread's been gone for a while, but I figured it's better I asked...

Nshanin mentioned strecker degradation. I looked it up and the rhodium link that appears shows the strecker degradation of alpha methyl dopa (http://www.erowid.org/archive/rhodium/chemistry/p2p.strecker.html). It turns into 3,4dihidroxyP2P. So what I'm wondering is, can you alpha methylate phenylalanine? If you could, it would then strecker degrade into P2P. Which would be awesome.

Oh, I also figured I'd add that the phenylalanine thread over at WD has brought up something called the akabori reaction. It's not directly related, but it says that you can react benzaldehyde with alanine in DMSO (with a little acetic acid) and get Phenylpropanolamine. Or, the benzaldehyde w/ N-methyl alanine to get ephedrine. I don't know much about this.

MrSparkle
2008-08-08, 22:02
UncleFester was going on about making Ephedrine with n-butyl-alanine (don't remember exact chemical but it was something like that) and benzaldehyde at wetdreams and I asked him what the hell he was talking about and other people backed up his claims. I looked into that n-butyl-whatever the fuck and it was far from OTC though.

hydroponichronic
2008-08-09, 08:17
UncleFester was going on about making Ephedrine with n-butyl-alanine (don't remember exact chemical but it was something like that) and benzaldehyde at wetdreams and I asked him what the hell he was talking about and other people backed up his claims. I looked into that n-butyl-whatever the fuck and it was far from OTC though.

N-Butyl? You don't mean N-Methyl alanine? If you do, monomethyaltion of an amine (and amino acids) occurs with this new formaldehyde/zinc thing. I don't know much about it, but its some new-ish reaction. Anyway, the good guys over at WD posted it somewhere in that thread. It was published tetrahedron letters 48 (2007) 7680-7682, if that helps. Well, anyway, I think you can make formaldehyde OTC with hexamine, but IDK. Anyone know anything about this? I just remember thinking that the Akabori synth is the greatest thing to happen to clandestine chemists since pseudophedrine.

fcknut
2008-08-09, 09:24
. It was published tetrahedron letters 48 (2007) 7680-7682, if that helps.

http://www.evilshare.com/ff463d64-b744-102b-a82a-00a0c993e9d6

stateofhack
2008-08-09, 14:49
I just remember thinking that the Akabori synth is the greatest thing to happen to clandestine chemists since pseudophedrine.

Indeed it nees some fine tunning but it works quite well. One word of warning. For the very final step your acetone has to be very very clean and dry, otherwise it will fuck up all your hard work :( trust me :(

hydroponichronic
2008-08-09, 23:46
Indeed it nees some fine tunning but it works quite well. One word of warning. For the very final step your acetone has to be very very clean and dry, otherwise it will fuck up all your hard work :( trust me :(

Final step? I have yet too see a write up for it. Do you know of one?

And while I'm asking, how clean? Dehydrated HW store Acetone not good enough?

stateofhack
2008-08-10, 01:39
Dehydrated HW store Acetone not good enough?

yeah its fine

nshanin
2008-08-10, 06:02
Nshanin mentioned strecker degradation. I looked it up and the rhodium link that appears shows the strecker degradation of alpha methyl dopa (http://www.erowid.org/archive/rhodium/chemistry/p2p.strecker.html). It turns into 3,4dihidroxyP2P. So what I'm wondering is, can you alpha methylate phenylalanine? If you could, it would then strecker degrade into P2P. Which would be awesome.

Unfortunately, no. Better chemists than you and me have tried to alpha-methylate raw phenethylamine, a very close relative to phenylalanine, without any success (though somebody somewhere mentioned using dimethylsulfate as a possible methylating agent, though I don't know of any reason that it would be more selective to the alpha carbon let alone reactive at all). What seems (to me at least) to be a far better idea would be to reduce the acid group on phenylalanine to an alcohol with LiAlH4, then oxidize to an aldehyde (still searching for an effective, cheap, and green way to do this, some ideas that I will research as soon as I can get free access to the articles, which will likely be on Monday: link (http://www.organic-chemistry.org/abstracts/literature/212.shtm), link (http://www.organic-chemistry.org/abstracts/lit1/020.shtm) (the iodine might make this one too suspicious :(), link (http://www.organic-chemistry.org/abstracts/literature/674.shtm)), then reduce via Huang-Milnon variation of Wolf-Kishner to obtain amphetamine (or the 3,4-dihydroxy derivative thereof when starting out with levodopa rather than phenylalanine. One concern to this though, l-dopa is only legal in 50% concentrations in the U.S., and even then it's expensive as hell. However, Chinese suppliers selling by the kilo are easily found on AliBaba<---this isn't sourcing, AliBaba might as well be Google).

If anybody has a relatively OTC method of reducing a primary alcohol (would RP/HI work? That's definitely not something I'd like to use but it would be interesting if possible), I'd love to see it, but so far my research hasn't turned up anything cheap or easy. Also, how hard would it be to buy some LiAlH4 (with luck, the only suspicious element of this synth) without raising eyebrows? I would assume it's common in the industry so it can't be watched that much, but I'm not completely familiar on this topic. Any help is appreciated.

stateofhack
2008-08-17, 20:49
However, Chinese suppliers selling by the kilo are easily found on AliBaba<---this isn't sourcing, AliBaba might as well be Google).

If anybody has a relatively OTC method of reducing a primary alcohol (would RP/HI work? That's definitely not something I'd like to use but it would be interesting if possible), I'd love to see it, but so far my research hasn't turned up anything cheap or easy. Also, how hard would it be to buy some LiAlH4 (with luck, the only suspicious element of this synth) without raising eyebrows? I would assume it's common in the industry so it can't be watched that much, but I'm not completely familiar on this topic. Any help is appreciated.

Be carefull with alibaba there is a lot of bullshit on there, i can tell you !:mad:

Either ways, that was a nice read and explanation there, so here is a little "help":

Buying LiAlH4 is a complete bitch (even in Europe), i don't in the US but with the nazi law i guess it can't be easy if not harder! . Your better of trying to buy it from a private person (who is willing) then from anywhere else. It is easier tho' to find and buy LiAlH4 in THF (pre maid "solutions"). As for it being watched well you better have a god damn good reason for it, because i believe it raises flags (i mean common, any use for the average person, not even home photo development uses this :( )
Your better of trying to find something else, even with a "license" the amount of paper crap for it is insane!
Ah and it is expensive too! and i doubt i need to remind you its a bitch to handle :(

nshanin
2008-08-17, 21:45
Hmmm, looks like it's back to the drawing board then. :( There aren't many easy ways to reduce acids without LiAlH, but I've researched a few ways of reducing the ester and amide derivatives, which is difficult and not OTC, but is still worth looking for. :mad: I just can't get over looking for a use for that acid group.

Did you get scammed on AliBaba? Anything specific I should look out for?

stateofhack
2008-08-17, 21:58
Hmmm, looks like it's back to the drawing board then. :( There aren't many easy ways to reduce acids without LiAlH, but I've researched a few ways of reducing the ester and amide derivatives, which is difficult and not OTC, but is still worth looking for. :mad: I just can't get over looking for a use for that acid group.

Did you get scammed on AliBaba? Anything specific I should look out for?

No i personally have not been scammed (yet) but there are quite a few other people who have (buying ketamine, idiots) and one person who i know personally got scammed buying NaBH4 on there :(

fcknut
2008-08-17, 22:53
There aren't many easy ways to reduce acids without LiAlH,

can't be fucked to look up refs, but acids can be reduced directly using borane (BH3), either neat, complexed with THF or DMS, or genertated in situ from NaBH4 and iodine...

Not strictly OTC, but there nonetheless...

stateofhack
2008-08-18, 10:00
can't be fucked to look up refs, but acids can be reduced directly using borane (BH3), either neat, complexed with THF or DMS, or genertated in situ from NaBH4 and iodine...

Not strictly OTC, but there nonetheless...

:o:o:o Please "be fucked" as what you just said is very very interesting! Please please please!!!

fcknut
2008-08-19, 10:08
:o:o:o Please "be fucked" as what you just said is very very interesting! Please please please!!!


Go on then, seeing as how you asked so nicely, even though I should really be doing some fucking work...!


http://www.evilshare.com/dddd8da0-bf26-102b-a14f-000b6aa2a5f8

stateofhack
2008-08-19, 11:56
Go on then, seeing as how you asked so nicely, even though I should really be doing some fucking work...!


http://www.evilshare.com/dddd8da0-bf26-102b-a14f-000b6aa2a5f8

I <3 you :) Let me read them and lets see what comes out of these!!