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Author: Subject: Amphetamine via ephedrine?
Filemon
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[*] posted on 26-4-2006 at 15:06
Amphetamine via ephedrine?


Is it possible to synthesize amphetamine with the method of Urushibara?

Ephedrine =======> Amphetamine
H2/U-Ni
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solo
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[*] posted on 26-4-2006 at 16:38


You might do well and visit Rhodium Archives and read up on it......solo

http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/




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[*] posted on 28-4-2006 at 07:31


My gut tells me with just Ni and H2 it needs lots of pressure, remembering Raney Ni did not work outside a bomb. OTOH: I remember that Al was used with the Urushibara Ni (not only to make it). Was that just for the H2 generation? But then again, they were not using ephedrine but P2NP. Thats from two of said files btw.
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[*] posted on 30-4-2006 at 08:39


I bet so. Have a look at:

http://www.google.com/search?hl=en&as_qdr=all&q=Urushibara+site%3Adesigner-drugs.com&btnG=Search

I think it's also possible with CTH - Raney Nickel (i-PrOH as the hydrogen donar). If these CTH procedures work for Raney-Nickel then I think they should also work for Ni-C or Urishibara-Nickel. I'm just guessing but it's definitely worth a try.

* Synth. Commun. 27, 817-23 (1997). Benzyl alcohol deoxygenation using CTH with Raney-Nickel.
http://designer-drugs.com/pte/12.162.180.114/dcd/pdf/cth.ra-...

* Applied Catalysis A: General 219 (2001) 281-289 : CTH using i-PrOH / Raney-Ni to reduce Benzylic alcohols.
http://designer-drugs.com/pte/12.162.180.114/dcd/pdf/ephedri...

Another route worth exploring could be Nickel Bromide.

* Chem. Commun., 2000, 1647-1648 : CTH using NiBr2
http://designer-drugs.com/pte/12.162.180.114/dcd/pdf/cth.nic...

Anyway this is what Rhodium wrote on the subject:

Quote:
Subject: (pseudo)Ephedrine to Meth w/ Raney-Nickel
Author: Rhodium (Chief Bee)
Date: 26-Dec-2002 21:23
Post No: 393077

(Rated as: excellent)

General procedure for Raney Ni catalyzed hydrogenolysis of aromatic alcohols
Applied Catalysis A: General 219, 281-289 (2001) (http://designer-drugs.com/pte/12.162.180.114/dcd/pdf/ephedri...)

1-Phenylethanol (2g) was added to a mixture of Raney nickel (5g) in 2-propanol (30 ml). While open to the atmosphere, the reaction mixture was vigorously stirred and refluxed (water-cooled condenser attached to flask) for 15 minutes. Isolation of the product involved decanting the 2-propanol solution, washing the Raney nickel with 2-propanol (3×10 ml), filtering the combined 2-propanol layers through celite, and evaporation of the 2-propanol and acetone to give ethylbenzene in 98% yield.

The yield is substantially the same with 1-Phenylethanol, 1-Phenylbutanol, 2,2-Dimethyl-1-phenyl-1-propanol and several other more or less sterically hindered alcohols, and both Raney Nickel and Raney Cobalt can be used as catalyst. The reaction is fast, clean, and uses simple isopropanol (IPA, 2-propanol) as the sole reducing agent (it turns into acetone) in conjunction with the catalyst. It is reasonable to believe that this reaction may work with Urushibara Nickel, and that (pseudo)ephedrine can be used as substrate to give methamphetamine.


Raney Ni catalyzed hydrogenolysis of (pseudo)Ephedrine amide to Methamphetamine amide
J. Org. Chem. 63, 7795-7804 (1998) (http://designer-drugs.com/pte/12.162.180.114/dcd/pdf/ephedri...)

To a mechanically stirred suspension of Raney Ni (wet, prepared from 200 g of aluminum-nickel alloy, Raney type Ni-Al 50:50) in ethanol (700 mL) was added 4 (29.55 g, 0.125 mol), and the mixture was heated to reflux for 2 h. After cooling to room temperature the mixture was filtered through Celite. Concentration, flash chromatography (hexane/ethyl acetate, 2:1) on silica gel (218g), and distillation (88°C/0.35 mmHg) gave 5 as a colorless liquid (23.80 g, 86%).

This is almost as close as it gets. In the article the authors describe that they did not have the proper licenses to synthesize methamphetamine, so they used very similar derivatives of ephedrine and pseudoephedrine (the ethoxycarbonyl amide) and reduced them to the ethoxycarbonyl amide of methamphetamine as the first step towards their target compound (which is completely unrelated). The yields for the ephedrine and pseudoephedrine amides were 86% and 81%, respectively, simply by refluxing them with freshly prepared Raney Nickel (Fieser & Fieser Vol. 1, p 729) in ethanol for two hours. Again, Urushibara Nickel might just work, and there is no glaring obstacle against using plain (pseudo)ephedrine instead of the corresponding amides, but this has not yet been tried in practice, and has been left as an exercise to the reader. Now you have something to do next year too, the Hive staff and elderbees always do their best to prevent you from getting bored...

Kudos to Foxy2 for finding these articles in the first place, and Happy New Year - whereever you are...
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Organikum
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[*] posted on 30-4-2006 at 09:42


Don´t waste time and money on this.

/ORG




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[*] posted on 2-6-2006 at 12:54
Raney does work


Not sure about urushibara but the raney/alcohol does work at atmospheric presure with decent yeilds.

A fellow on ebay sells 500g. for $85 american
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[*] posted on 8-6-2006 at 11:16


Quote:
Originally posted by Organikum
Don´t waste time and money on this.

/ORG


agreed

in another way you can get meth from benzhaldehyde ,some base catalyst and NaNO2

but meth= poison

so , "solo" youre drug dealer or what??? you always are interested on drug articles....fuckin fagget
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[*] posted on 8-6-2006 at 12:37


Quote:

"solo" youre drug dealer or what??? you always are interested on drug articles....fuckin fagget


..............what did I do to you to deserve your insolence and bad manners..........solo




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[*] posted on 8-6-2006 at 12:46


andres = troll
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[*] posted on 8-6-2006 at 21:20


Quote:
Originally posted by solo
Quote:

"solo" youre drug dealer or what??? you always are interested on drug articles....fuckin fagget


..............what did I do to you to deserve your insolence and bad manners..........solo


i did hit in the spot?? lol , youre pathetic , i ll to uncover u silly dealer
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[*] posted on 8-6-2006 at 21:47


andreseris, if u keep being such a fagget i will ban u.

lol.

im serious.




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[*] posted on 8-6-2006 at 22:40


Here's a link from totse (Accuracy not ensured):
http://www.totse.com/en/drugs/speedy_drugs/hydrogeniodide191...

Here's a link for amphetamine via a different method:
http://www.erowid.org/archive/rhodium/chemistry/amph.alhg.ht...
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[*] posted on 8-6-2006 at 22:52


It is possible as cherrybaby pointed out it can be used to reduce benzylic alcohol, but somethings will have to be changed; such as temperature, solvent, and whatever else when trying to reduce ephedrine. But then it is also a waste of time and effort unless your doing it for the pure science, you will have trial and errors.

[Edited on 9-6-2006 by chochu3]




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[*] posted on 11-6-2006 at 00:54


As for the Raney part of this which came up, these dudes
http://www.erowid.org/archive/rhodium/chemistry/nor-pseudo-e...
hydrogenated at high pressure and although they do not exactly say "until hydrogen uptake ceased", it does seem to be implied that the reduction went no further than the alcohol in both cases. It is interesting to compare this to the earlier US2243295 by the same author, the results being completely different.
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