Author Topic: reduction of L-PAC to Meth  (Read 8700 times)

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onevegasdave

  • Guest
reduction of L-PAC to Meth
« on: May 01, 2004, 03:10:00 PM »
Swim has produced about 100g of L-PAC with the help of freindly Bee's...now the reduction to Meth is a little confusing. Which is the preferred meth of reduction of the Bees that have done the L-Pac reduction. Comments, criticisms are welcomed


ChemoSabe

  • Guest
Organikum L-PAC
« Reply #1 on: May 01, 2004, 03:23:00 PM »
All I can say is that you might find out with a search of Organikum & L-PAC

Good luck and congrats on the L-PAC production. It's the real wave of the future. Fuck pill extraction.

methylamine is another keyword that might get you somewhere


DrLucifer

  • Guest
l-pac
« Reply #2 on: May 02, 2004, 01:08:00 AM »
You will need to reductively aminate the raw l-pac juice to get l-ephedrine. From there, the path to meth is your preferred choice obviously.
I havn't performed the bio-synth, but i hear the al/hg reduction is a preferred method.
If you dont mind, i have a few questions.
Did you treat your yeast with acid prior to fermentation?
What combination of nutrients did you utilise?
How much benzaldehyde did you add to obtain 100g?
Cheers, and congrats, i wish you luck  :)


Organikum

  • Guest
Benzaldehyde -> L-PAC -> Ephedrine
« Reply #3 on: May 06, 2004, 03:44:00 AM »
The article he spoke of is probably:

Biotransformation of benzaldehyde to l-phenylacetylcarbinol (l-PAC) by Torulaspora delbrueckii and conversion to ephedrine by microwave radiation
J. Technol. Biotechnol. 77, 137-140 (2002) DOI:

10.1002/jctb.534





The article deals with the usual biosynthesis followed by microwave supported imine formation and reduction of the imine by NaBH4 in a microwave.

The claimed yields of the biosynthesis are to good to be true (maybe the are true but the technical effort is immense), the yields of the imine formation are lousy and the yields in the final NaBH4 reduction are ok.
A modificated household microwave oven was used.

btw. of course all reductive alkylations of l-PAC with methylamine end with ephedrine - what else?


amalgum

  • Guest
One speculation SWIM has had in the past is...
« Reply #4 on: May 06, 2004, 04:25:00 AM »
One speculation SWIM has had in the past is reduction of an imine formed between an l-pac ester and methylamine, to proceed straight to meth.

Would it be possible to somehow esterfy the alcohol group without disturbing the keto group (including ways to protect/de-protect the keto group) wich would allow proper imine formation when reacted with methylamine without fucking up the ester group (damn did I even word that right?)?  Lets say for examples sake the l-PAC was reacted with acetic anhydride to make acetic ester of the alcohol group.  Then that was added to an alcohol and gassed with methylamine to form the imine, then followed up with say Pd/C-ammonium formate reflux, reducing both imine and ester, turning imine to amine and removing the alcohol all at the same time proceeding directly to meth.

Is anything like that even remotely possible?

Organikum

  • Guest
A reduction of the preformed imine under ...
« Reply #5 on: May 06, 2004, 04:39:00 AM »
A reduction of the preformed imine under (strong) acidic conditions with a powerful reducing agent (maybe Al/HG suffices, Pt/Pd will) should produce methamphetamine directly.
Hydroxyphenylacetones form stable imines, so the there is no attackable keto-group left. The hydroxy group of the imine is told to be prone to reduction in acidic environment - thats why usually alkaline conditions are used - to suppress the reduction of the -OH.
Not to forget: The pathway l-PAC - ephedrine - meth is not straightforward but more two steps forward and one back, this is also true if done as "one pot" reaction.


amalgum

  • Guest
Re: A reduction of the preformed imine under...
« Reply #6 on: May 06, 2004, 02:45:00 PM »


A reduction of the preformed imine under (strong) acidic conditions with a powerful reducing agent (maybe Al/HG suffices, Pt/Pd will) should produce methamphetamine directly.




You think so?  Like maybe a conglomeration of the catalytic hydrogenation methods for ephedrine with Pd catalyst and acid promoter (like H2SO4 or HClO4).  Maybe preform the imine in alcohol, add Pd/C bring to reflux and slowly add the NH4COOH over time.  When reduction of the imine is complete, maybe one could just cool it down, add acid and maybe some fresh catalyst, bring back to reflux and add more formate for reduction of the alcohol group (damn that was a long run on sentence).



Hydroxyphenylacetones form stable imines, so the there is no attackable keto-group left.




Yeah SWIM knows, what SWIM meant was will ESTERFICATION of some sort attack the keto group before imine formation.  SWIM knows halogenation is probably out of the question as any halogenic acids will cause condensation of the ketone (if SWIM remembers correctly from reading about making phenylmethylbutenone from MEK and benzaldehyde).  But SWIM forgot all about those catalytic hydrogenation documents for ephedrine that use acid promoter and Pd or Pt catalysts using straight ephedrine (no ester) as precursor.  So it seems apparent that no esterfication would be required anyway (for a one pot reduction anyhow).



Not to forget: The pathway l-PAC - ephedrine - meth is not straightforward but more two steps forward and one back, this is also true if done as "one pot" reaction.




What exactly do you mean?


Man if a one pot method can be developed, then like someone said above this pathway may very well be the wave of the future.  SWIM is gonna have to tinker with this idea now.  Now SWIM needs some benzaldehyde.....hrmmm.  SWIM was always partial to the akabori process however, but has never tried it so only knows how it would work in theory.  The speculations above are still only theory, and we all know chemistry more often than not deviates from theory (in reality that is).

Man I love this website.  All we need is a bunch of smart chemists to keep on callaborating, and the drug war will never be won!  I mean as far as meth goes, we could make it from styrofoam cups and vinegar for christ sake (talk about starting from scratch!)!  Are they gonna control those two?


borolithium

  • Guest
Borohydride reduction of L-PAC
« Reply #7 on: May 06, 2004, 08:45:00 PM »
- The claimed yields of the biosynthesis are to good to be true (maybe the are true but the technical effort is immense), the yields of the imine formation are lousy and the yields in the final NaBH4 reduction are ok.
A modificated household microwave oven was used.


I have read in the serious chemistry forum that the reductive amination of L-PAC to ephed is almost identical to the MDP2P aminations and that any of those techniques can be applied to the L-PAC.

With MDP2P, the borohydride reduction is very exothermic, requiring heavy cooling and slow additions of the borohydride over several hours under strong stirring. If cooled sufficiently, it is also high yielding.

 Is this not the case with the L-PAC reduction? Does the reaction require energy from microwave radiation to proceed?

The borohydride reduction appears to be the best way to produce ephed in large quantities, as it is quite scalable and the availability of sodium borohydride is becoming more and more available, not only as an alternative energy source, but also for pulp and paper mills and waste water management. The HG/Al amalgamation on the other hand generates a lot of toxic waste and is better for small scale operations. I would imagine it is much harder to obtain mercury salts in large quantities and you may need to hire someone full time to cut up pie plates! If you're sloppy, enjoy the permament brain damage!

Raney nickel is a pain in the ass to get as well I understand.


Organikum

  • Guest
Yes, of course , all methods which work for...
« Reply #8 on: May 07, 2004, 01:30:00 AM »
Yes, of course , all methods which work for P2P or MDP2P will work for l-PAC too. But l-Pac has also the option of preforming a stable imine what doesnt apply for P2P and MDP2P.


amalgum

  • Guest
Re: But l-Pac has also the option of ...
« Reply #9 on: May 07, 2004, 02:03:00 PM »


But l-Pac has also the option of preforming a stable imine




Heh, thats music to swims ears!


borolithium

  • Guest
Pardon My NewBee Ignorance
« Reply #10 on: May 07, 2004, 06:49:00 PM »
Organikum, what exactly does that mean to us in the scheme of things?


Organikum

  • Guest
Re: Organikum, what exactly does that mean to...
« Reply #11 on: May 08, 2004, 01:38:00 AM »

Organikum, what exactly does that mean to us in the scheme of things?



This says that there is a realistic chance that it is possible to form the imine from l-PAC by adding methylamine (called condensation) and to reduce this imine straight through to methamphetamine. Acidic conditions and a powerful reducing agent will be needed - Al/Hg maybee, Zn/HCl, or best noble metal catalysts (Pt/Pd). Maybe other catalysts might work too (H2S/HI), this I dont know.
Nevertheless there is strong evidence that the hydroxyl-group of an imine is easier reduced than the hydroxyl-group of the amine.




amalgum

  • Guest
Hehe, add methylamine HCl to some methanol and
« Reply #12 on: May 08, 2004, 02:21:00 PM »
Hehe, add methylamine HCl to some methanol and add equal molar amount of lye, filter off NaCl that precips.  Throw on mag stirrer, and drip in l-PAC.  From there, can someone say microwave assisted Pd/C with ammonium formate for reduction.  Imine first, then add promoter acid and kick off that hydroxyl.  Easy as pie.  SWIM hopes this proves viable.

borolithium

  • Guest
But,,,,
« Reply #13 on: May 08, 2004, 08:17:00 PM »
The lye additions to the methylamine hydrochloride will produce a fair bit of water. Won't that interfere with the reaction?

It would seem better to me if one used dry methanol and bubble methylamine gas through a drying tube of Magnesium Sulphate, then into a -20C solution, by liberating the methylamine HCL in a seperate vessel.

I would seem to think water is not a good thing in this type of reaction. Am I wrong?


amalgum

  • Guest
It would be overkill to do all that drying.
« Reply #14 on: May 08, 2004, 10:08:00 PM »
It would be overkill to do all that drying.  When an imine gets formed, water is formed as a byproduct anyway which never seemed to hurt reduction (of the imine to amine least), esp. the Pd/C with NH4COOH reflux.  SWIM doesn't think it would hurt reduction of the hydroxyl group either as it is most often reduced in an aqueous environment (look at HI/P reductions of ephedrine).

BOS

  • Guest
Another patent
« Reply #15 on: May 10, 2004, 06:26:00 AM »

Patent WO03018531


Carry on from Co2 patent posted by Roger2003

This is an interesting read if not for only showing possibilities.

Not much use to the home handy man, but does touch upon reducing PAC to Meth etc.

Organikum

  • Guest
Re: but does touch upon reducing PAC to Meth...
« Reply #16 on: May 10, 2004, 07:56:00 AM »

but does touch upon reducing PAC to Meth


where please?




Rhodium

  • Guest
Benzaldehyde -> L-PAC -> PPA
« Reply #17 on: May 18, 2004, 09:18:00 AM »
Synthesis of (1RS,2SR)-(±)-2-Amino-1-phenyl-1-propanol from (R)-(-)-1-Hydroxy-1-phenyl-2-propanone
Prema M. Subramanian, Sunil K. Chatterjee and Mahesh C. Bhatia

J. Chem. Tech. Biotechnol. 39, 215-218 (1987)

(https://www.thevespiary.org/rhodium/Rhodium/chemistry/ppa.l-pac.raney-ni.html)

Abstract
Synthesis of (1RS,2SR)-(±)-2-amino-1-phenyl-1-propanol (2) by reductive amination of (R)-(-)-1-hydroxy-1-phenyl-2-propanone (1) using ammonia and Raney nickel as a catalyst was investigated. Compound 1 was produced by fermentation of molasses with a strain of yeast and benzaldehyde was added during the course of fermentation.

Also see

Post 44728 (missing)

(LaBTop: "Patent Collection: L-PAC Synthesis", Stimulants)



aia2

  • Guest
Where can we go from our L-PAC?
« Reply #18 on: June 24, 2004, 03:38:00 PM »

where please?




The "SUMMARY OF THE INVENTION" includes the following:

According to one embodiment of the invention, the amine (VI) is selected from the group consisting of ephedrine (R4 = OH, R5 = phenyl, R2 = methyl, R6 = R3 methyl), isoetharine (R4 = OH, R5 = 3,4-dihydroxyphenyl, R2 = ethyl, R6 = R3 = isopropyl), ritodrine (R4 = OH, R5 = 4- hydroxyphenyl, R2 = methyl, R6 = R3 = 2- (4- hydroxyphenyl) ethyl), methamphetamine (R4 = H, R5 = phenyl, R2 = methyl, R6 = R3 = methyl), fenfluramine (R4 = H, R5 = 3-trifluoromethylphenyl, R2 = methyl, R6=R3= ethyl) and propylhexedrine (R4 = H, R5 = cyclohexyl, R2 = methyl, R6 R3 = methyl). These compounds are preferably formed using hydrogen and a catalyst as the reductant, although they can be formed using a hydride reducing agent.

According to an alternative embodiment of the invention, the amine (VI) is selected from the group consisting of amphetamine, methoxamine, phenylpropanolamine, hydroxyamphetamine, ethylnorepinepherine and metaraminol. These compounds may be formed using a hydride reducing agent as the reductant.


I'm a Newbee, so please forgive and correct my errors.  The imine that is formed from the L-PAC is 2-(methylamino)-1-phenyl-1-propanol, which needs to be reduced twice to get to methamphetamine.  However, it looks to me like there will be ephedrine in situ because it is the result of a single reduction.  How is this taking two steps forward and one step back?

Another question, why should this be done under strong acidic conditions?




ChemoSabe

  • Guest
L-Pac Questions
« Reply #19 on: June 24, 2004, 08:48:00 PM »
aia2 axed...

Another question, why should this be done under strong acidic conditions?

I think Orgy somewhat covered this in one of his posts above by stating...

Hydroxyphenylacetones form stable imines, so the there is no attackable keto-group left. The hydroxy group of the imine is told to be prone to reduction in acidic environment - thats why usually alkaline conditions are used - to suppress the reduction of the -OH.

I really don't get your first question but if it's what I think it it is the answer is  just be happy enough that you didn't have to deal with pill extraction.