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Author: Subject: Catalytic Hydrogenation
zed
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[*] posted on 11-10-2008 at 21:57


Ah, my memory IS accurate after all. I recalled, that About forty years ago, my buddy Alex Palmiter (RIP), told me about his preferred method of making Methamphetamine from Ephedrine. It was reacting the alcoholic functional group of Ephedrine with Thionyl Chloride and reducing the resultant 1-chloro-1-phenyl-N-methyl-isopropylamine to Methamphetamine via Hydrogenation.

Oddly enough, at that time, making Meth was very illegal, and in most quarters it was considered highly immoral. How times have changed. (Sarcasm)

Anyway, there is an interesting reference to this method on the DEA's "Microgram" website. A place I like to visit occasionally, as a reality check. I sometimes forget how stressful the game of cops and clandestine chemists, actually is.

http://www.usdoj.gov/dea/programs/forensicsci/microgram/mg04...

Oh man! Caught in lab with 28 Kilos of Meth. That has to rate some serious prison time.


[Edited on 11-10-2008 by zed]
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JohnWW
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[*] posted on 12-10-2008 at 03:30


Or some serious bribery! The DEA is as corrupt as hell.
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zed
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[*] posted on 13-10-2008 at 02:09


John,

Microgram is a website constructed by the U.S. DEA. And, while men are mere flesh, and thereby are corruptible......Here in the States, in general, if the DEA has a good case against you, you will not be bribing your way out of trouble.

Across our Southern Border in Mexico, dealers can hire platoons of Federales, to guard their drug shipments during transport. Not so in the U.S..

That being said, the aforementioned link is full of tasty tidbits of information....Like, how much meth the Mexican Mafia smuggled into California, last year.....And, How adultrated common illegal drugs are, and with what.

Also full of mystery. Why were these Asian chemists intentionally making L-Methamphetamine? Is this material superior in some way to the supposedly stronger D-Methamphetamine? I do not plan to make any, but it makes you think.
What were they up to?

And, since this is a link on catalytic hydrogenation......Of further interest, was their non-chalantly mentioning "Activatiing" the substrate via Nitric Acid or Sodium Acetate. I did not know of those methods.
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[*] posted on 13-10-2008 at 03:28


Are catalytic hydrogenations better suited when shaken or stirred?
Since when using certain catalyst they can auto ignite if not dilute maybe im going down the stir path. Anyone had experience with the stirring instead of shaken?
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stoichiometric_steve
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[*] posted on 13-10-2008 at 14:11


Quote:
Originally posted by zedWhy were these Asian chemists intentionally making L-Methamphetamine?


They obviously didnt know that their precursor was the wrong stuff ;)

Alternatively, they were trying to make some Vicks inhalers.




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zed
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[*] posted on 13-10-2008 at 18:34


Steve,

With a 30 liter Hydrogenator, and 28 kilos of product? Not likely. I'm inclined to think that those boys knew something that we don't.

Shaken, not Stirred?,

Either method works fine. Purge all air from the system and both work well. Many catalysts are pyrophoric however. The activated catalyst is full of adsorbed hydrogen. And, If you allow such a catalyst to dry out while in contact with air, that hydrogen will react with atmospheric O2, the catalyst will become very hot, and it will ignite itself and any nearby solvent. Might even cause an explosion. This is a bad thing.

Read up on the perils of such procedures. Even better, take a class, or find a mentor who is experienced with the relevant equipment.
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[*] posted on 13-10-2008 at 19:20


I seriously doubt that Zed! The vast majority of these guys are far from rocket scientists and even less so, real chemists. There are no new unknown qualities of l-meth to be discovered. Don't you think the pharma industry has ben giving speed in all possible shapes and form to humans and animals alike in enough number of doses to make it perfectly clear which form gives you the best bang for your buck? Christ it has been known for about 120 years.

A stirred reactor always beats a shaken reactor in saturating the catalyst with hydrogen. By keeping the catalyst as saturated with hydrogen as possible less unwanted side reactions will occur.
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stoichiometric_steve
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[*] posted on 13-10-2008 at 23:37


And i'm inclined to think that these boys were just well trained, look at the product...

Apart from that, i have to agree with Barium. I have never done meth but for me and the various pharmacopoeias, the L-form is a vasoconstrictor and thats it.




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[*] posted on 14-10-2008 at 01:20


I will investigate this matter. I have heard counter claims.

Pause........

Well, I'm back. There were very interesting discussions on L versus D, versus D-L , out on the web.

For the moment, I'm going to surmise that those Asian chemists weren't through.

Has it occurred to you that those "wrong" isomers might be OTC in some parts of the world, and the chemists might have intended to racemize that L-Metamphetamine into D, L, Methamphetamine, via a further reaction?



[Edited on 14-10-2008 by zed]
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[*] posted on 14-10-2008 at 04:01


Then why the trouble to recrystallize the product to make the "ice" appearance? Nah, those idiots simply had no clue about chirality. Then again, speed cooks aren't the top of the evolutionary ladder. And for the love of God Zed, calling them chemists is an insult to chemistry.
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[*] posted on 14-10-2008 at 06:18


...................I'd say they are in the business of making cut.....since it will crystallize and look like the d-isomer ...otherwise they would need the free base to either work it back to P2P or to do a metal recimization....but then who knows what their motive might be save use it as a pure chiral to help resolve something of more value to them......solo



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[*] posted on 10-1-2009 at 19:10


Quote:
Originally posted by zed


And, since this is a link on catalytic hydrogenation......Of further interest, was their non-chalantly mentioning "Activatiing" the substrate via Nitric Acid or Sodium Acetate. I did not know of those methods.


....does that mean they will recimize using those methods of activation .....the talk is refluxing the l,isomer with 37% HCl for 14 hours will recimize the isomer be it l, or d.....which is much easier than the involved pd. `zinc, iron to make a metal mix to do the recimization as noted on `patent -Recemization`- `improved method for converting l. amphetamine to d,l. amphetamine-pat-US2797243....`i would be interested if anyone has a working method to recimize active isomers besides those mentioned......solo




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[*] posted on 21-9-2009 at 22:34


Quote: Originally posted by solo  
Quote:
Originally posted by zed


....does that mean they will recimize using those methods of activation .....the talk is refluxing the l,isomer with 37% HCl for 14 hours will recimize the isomer be it l, or d.....which is much easier than the involved pd. `zinc, iron to make a metal mix to do the recimization as noted on `patent -Recemization`- `improved method for converting l. amphetamine to d,l. amphetamine-pat-US2797243....`i would be interested if anyone has a working method to recimize active isomers besides those mentioned......solo


Are you sure about the information of racemizing l isomer with 37% HCL for 14 hours its true??:o
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[*] posted on 27-12-2009 at 09:41


......nothing is sure till it's tried, but i think the amine has to be in a phase transfer solvent such as acetone ...and in such a case perhaps an alkaline environment would work best as done with amides in patent US4918196.....solo



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