Author Topic: L-PAC -> Reductive Amination to Ephedrine (Read 394 times)

bobr · « **on:** October 13, 2010, 03:35:40 PM »

HI all,

any idea how to make subject from L-PAC ? I try this:

Phenylacetylcarbinol (0.2 g, 1.3 mmol), palladium catalyst (0.05 g) and 5 fold excess of 2.0M methylamine in THF (3.125 mls, 6.45 mmol) was then placed into the stainless steel pressure vessel. The vessel was pressurised up to 400 psi withhydrogen gas and then up to a total of 1500 psi by pumping dried liquid carbon dioxide into the vessel. The vessel was then stirred in a 35° C. water bath for 24 h. After 24 h, the reaction vessel was cooled to room temperature and slowlyde-gassed. The vessel contents and residue was washed three times with diethyl ether and filtered. Gas chromatography analysis revealed 60% conversion of phenylacetylcarbinol (PAC) to ephedrine.

But the price for methylamine in THF its very high

, have somebody other method ??

th. all for reply

embezzler · « **Reply #1 on:** October 13, 2010, 03:47:45 PM »

Seems you have access to chems so this may help:

If nothing else it give good background info:

Manufacturing by-products from, and stereochemical outcomes of the
biotransformation of benzaldehyde used in the synthesis of methamphetamine

Matthew Cox a, *, Gunter Klass b, Christina Wei Min Koo b

Forensic Science International 189 (2009) 60–67
doi:10.1016/j.forsciint.2009.04.010

ABSTRACT
Clandestine synthesis of methamphetamine in Australia has predominantly started from pseudoephe-drine extracted from over the counter cold and ?u medications. However, recently introduced restrictions on the sale of these products havemade pseudoephedrinemuchmore dif?cult to obtain. As a result clandestine chemists have had to resort to other means of obtaining the necessary chemical precursors. A recent drug raid (Adelaide, January 2008) resulted in the seizure of an unusual reaction mixture that indicated a novel approach involving the fermentation of glucose by yeast in the presence of benzaldehyde to give 1-hydroxy-1-phenylpropanone, also known as l-phenylacetylcarbinol (l-PAC), a known precursor to ephedrine and pseudoephedrine and hence methamphetamine. A study was undertaken into this process with the aim of determining the characteristic reaction by-products associated with methamphetamine made in this way. The study also looked at the stereochemical selectivity of the fermentation reaction and the stereochemistry of the subsequent reaction products,
ephedrine and pseudoephedrine, and the ?nal methamphetamine.

Keywords:
l-PAC, Biotransformation, Methamphetamine, Chirality, Ephedrine

embezzler · « **Reply #2 on:** October 13, 2010, 08:05:28 PM »

By any chance does anyone have Organikum's Hive posts on L-pac?

jon · « **Reply #3 on:** October 13, 2010, 08:19:22 PM »

just follow him around at SM he seemed to prefer aluminum amalgum over this shit.
another note brew the laevopheylacetyl-1-carbinol using malt extract it seems to need those plant enzymes to actually work.
the patents will mislead you.

bobr · « **Reply #4 on:** October 14, 2010, 04:07:20 PM »

Hi to all,

its here somebody who want speak real, or its this forum only for speak shit ?? I looking for good way to make subject, with all information like i send

embezzler · « **Reply #5 on:** October 14, 2010, 04:31:28 PM »

Hey...

I am all for the discussion and there is a different procedure in the journal I uploaded for you. Do you know if the bioconversion of benzaldehyde works with substituted benzaldehyde?

lugh · « **Reply #6 on:** October 15, 2010, 02:12:46 AM »

Quote

Do you know if the bioconversion of benzaldehyde works with substituted benzaldehyde?

According to reference thirteen in the FSI article it's possible :

H. Ohta, K. Ozaki, J. Konishi, G.-i. Tsuchihashi, Reductive C2-homologation of substituted benzaldehydes by fermenting Baker’s yeast, Agric. Biol. Chem. 50 (1986) 1261–1266.

embezzler · « **Reply #7 on:** October 15, 2010, 03:12:28 PM »

You dont expect me to read refs all the way to the end do you Lugh

Just scanning this the percentage conversions are not great but still its one to keep in the old memory banks.

A free download is available from here:

hxxp://www.journalarchive.jst.go.jp/english/jnlabstract_en.php?cdjournal=bbb1961&cdvol=50&noissue=5&startpage=1261

bobr · « **Reply #8 on:** October 18, 2010, 09:54:25 AM »

Hi all,

th. for yours posts, but i lookin for reductive animation (hydrogenation) L-PAC to ephe, not how to make L-PAC ( i have good quality source )

any other idea ??

/bobr

bobr · « **Reply #9 on:** December 16, 2010, 03:42:39 PM »

Hi all,

we finish the hydrogenation, and i have one question, how to wash the contents and residue with diethyl ether ?? Please step-by-step

/Bobr

akcom · « **Reply #10 on:** December 16, 2010, 05:03:32 PM »

You mean you were able to use a hydrogenation vessel but you don't know how to wash with diethyl ether? I'm worried for your neighbors.

bobr · « **Reply #11 on:** December 16, 2010, 07:04:44 PM »

HI,

don`t wory and reply me

. Its easy to use hydrogenation vessel, but i don`t have any experience about ether, then give me answer please to me question

th.

/bobr

lugh · « **Reply #12 on:** December 17, 2010, 12:35:16 PM »

Reading these documents may help in increasing your understanding, clearly you need to study the subject more thoroughly

There is a lot of information available online about your question such as:

http://library.sciencemadness.org/library/index.html

You need to study the subject instead of expecting spoon feeding

All you did was cut and paste what you posted, the result comes from the effort applied

Vesp · « **Reply #13 on:** December 17, 2010, 08:45:35 PM »

While this topic has some good information in the references, the discussion isn't of the quality The Vespiary aims for when it comes to forum discussion.

I realize there is some language barrier, but there is a clear lack of attempted research and the original poster is unclear/vague on what they have actually done and are trying to accomplish.
Please review the rules, here: http://127.0.0.1/talk/index.php/topic,369.0.html

Quote

When making a new thread in Drug Synthesis & Extraction, Other Chemistry, and Pharmacology - and preferably others if applicable show that you have researched, and have searched here on the site by providing links and references of relevant information, or at least mention how you cannot find any detail related to the subject in which you are posting.

I am now going to lock this thread before it gets out of hand.

Author Topic: L-PAC -> Reductive Amination to Ephedrine (Read 394 times)

bobr

L-PAC -> Reductive Amination to Ephedrine

embezzler

Re: Reductive Amination to Ephedrine

embezzler

Re: L-PAC -> Reductive Amination to Ephedrine

jon

Re: L-PAC -> Reductive Amination to Ephedrine

bobr

Re: L-PAC -> Reductive Amination to Ephedrine

embezzler

Re: L-PAC -> Reductive Amination to Ephedrine

lugh

Re: L-PAC -> Reductive Amination to Ephedrine

embezzler

Re: L-PAC -> Reductive Amination to Ephedrine

bobr

Re: L-PAC -> Reductive Amination to Ephedrine

bobr

Re: L-PAC -> Reductive Amination to Ephedrine

akcom

Re: L-PAC -> Reductive Amination to Ephedrine

bobr

Re: L-PAC -> Reductive Amination to Ephedrine

lugh

Re: L-PAC -> Reductive Amination to Ephedrine

Vesp

Re: L-PAC -> Reductive Amination to Ephedrine