Rhodium (Chief Bee)
07-28-01 19:11
No 199561
      Forensics find an unusual meth synthesis in NZ  Bookmark   

AN UNUSUAL METHOD OF METHAMPHETAMINE MANUFACTURE IN NEW ZEALAND

Wayne Gatenby

ESR, Private Bag 92021, Auckland, New Zealand

An unusual method of manufacture of methamphetamine has recently been encountered in New Zealand. The method involved an attempted production of methamphetamine from organomagnesium compounds (Grignard reagents). The process involved three steps. The first step being the reaction of benzyl chloride with magnesium to form a Grignard reagent. Methylamine and acetaldehyde were then reacted to form N-methylacetaldimine which was reacted with the above Grignard reagent to produce methamphetamine.

What makes this method even more unusual is that the benzyl chloride, methylamine and acetaldehyde were not commercial products, but were being manufactured from simpler chemicals. The process used chemicals that are not restricted in New Zealand, although it is relatively difficult to synthesise methamphetamine by this method.

../rhodium
 
 
 
 
    Semtexium
(Hive Elder)
07-28-01 19:39
No 199563
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Sad to see someone actually tried to circumvent the fucked up drug laws in that country and got caught.  It seems that they were well aware of watched chems and such and there was at least some thought put into the production since it didn't use anything restricted even though doing so required more steps in the process.  I've heard the prices for drugs in NZ are just fucking insane though, no idea how much meth was being produced...?

crazylaughsmiletonguewink    Mean People Suck    winktonguesmilelaughcrazy
 
 
 
 
    lunatic_asylum
(Stranger)
07-29-01 01:54
No 199623
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Its just the same method as mentioned in Gazetta Chimica Italiana, Vol. 77 (1947) p.318
 
 
 
 
    Rhodium
(Chief Bee)
07-29-01 03:24
No 199642
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Yup, has anyone found that article in full text and translated it to english yet?

../rhodium
 
 
 
 
    obituary
(Hive Addict)
07-29-01 03:34
No 199645
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

might it look similar to this: ../rhodium/chemistry /grignardimine.html    ?

this is the full synthesis by that method.  maybe the article you request has different details involved or you're just looking for more info, but it seems pretty straight forward from this direction.
 
 
 
 
    Rhodium
(Chief Bee)
07-29-01 04:18
No 199656
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

I just wanted to read the original article, as the stuff written in that text on my page was gathered from several different posts at the old hive (the diagrams added by myself) and this was about the only thing that guy posted, and he has disappeared since. I was looking for more non-anecdotal information on the actual reaction.

If it works as simply as stated, it is a mystery why this method isn't more extensively used. It is all OTC, too (benzyl chloride from toluene/bleach, methylamine from hexamine/HCl, and acetaldehyde from the oxidation of ethanol).

../rhodium
 
 
 
 
    ChemGrrl
(Guilty of Contempt)
07-29-01 05:14
No 199664
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

It looks good, the thing is, it requires too much baby-sitting and tlc from the chemist running the process.

Most Norte Americano kids don't have that patience or discipline.  And hell, if they keep the federales running around harrassing farriers, pool supply retailers and match companies, then the federales won't recognize what is going on when they shine the flashlight in the car on the way home from a shopping trip.

vive la resistance!

ChemGrrl

Six legs good, four legs food.  (pigs 4, sheep 4, bees 6)
 
 
 
 
    jim
(Hive Bee)
07-29-01 08:39
No 199707
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

THis method is tempermental.  As are all Grignard reactions.  Imagine the some Yahoo trying to use dirty Mg, or wet ether... Oh the agony.

I can imagine that if you were clever enough you could put together quite a patch work of syntheses to make this work.

As a personal addition to this synthesis I would make the benzyl chloride from Ca(OCl)2 and toluene, not separate the benzyl chloride from the unreacted toluene, and use my post "Gringard reactions in solvents other than ether" as a guide line.

I would also definitely add the Grignard reagent, C6H5CH2-Mg-Cl, to the acetlyhyde, thus first quenching the Grignard reagent with the first order reaction, and thus negating alcohol formation.

 
 
 
 
    WizardX
(Wizard Master)
08-07-01 06:14
No 202029
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Yes! Yes! I have mentioned this synthesis may times. That's why benzyl chloride is HIGHLY RESTRICTED.
Also, benzyl chloride + acetic anhydride => P2P.
 
 
 
 
    obituary
(Hive Addict)
08-07-01 07:04
No 202042
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

is that so, what ratio? any rxn conditions?
 
 
 
 
    Rhodium
(Chief Bee)
08-07-01 15:52
No 202151
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

From phenylacetone.html at my page:

P2P from Benzylchloride (via Dibenzyl zinc)

This is all quite interesting but the dibenzyl zinc or dibenzyl cadmium route is much better and much quicker with no dimerization and no catalysts needed Add a slight excess of Mg to freshly dried/distilled benzyl chloride (vapor phase thru anhydrous CaCl2 will do nicely) in about 3x mol. of dry Et2O or THF add 1/2 equiv of freshly dried Zinc chloride or Cadmium Chloride as quickly as possible while still keeping things halfway tame (don't overun the reflux) When reaction has subsided add one equiv. acetic anhydride dropwise until reaction is finished. Quench in dilute HCl/ice water - yield 80~90%


I would love to have the references for this reaction.
 
 
 
 
    Rhodium
(Chief Bee)
08-09-01 02:49
No 202650
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

I have now translated the original italian article for the reaction used in the lab mentioned at the top: Post 202649 (Rhodium: "Meth via grignard rxn (Gazz Chim Italiana)", Novel Discourse)
 
 
 
 
    tecnetium
(Hive Bee)
08-21-01 05:30
No 206198
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Dibenzyl zinc + Ac2O -> P2P = great little synth! Must have clean/pure/dry reagents though. Rhodium- did you ever find out how that poor chump in NZ got busted in the first place? Neighbours? Ordering non restricted chems with his own name? Someone n the know lagging on him'?
 
 
 
 
    goiterjoe
(Hive Addict)
08-21-01 07:27
No 206224
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

even sadder is the fact that he probably didn't make any product.  The article said he was attempting to make meth via this reaction, not that he was manufacturing using this reaction.

Drunk driving, that's what I like to do,
I like drunk driving with you.
 
 
 
 
    Rhodium
(Chief Bee)
08-21-01 14:30
No 206278
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

The only info I've got is the article at the top.
 
 
 
 
    joyman
(Stranger)
10-28-01 10:38
No 229535
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

Hey tecnetium!

What was your conclusion with

1) bzMgcl + ZnCl -> dibenzyl zinc
2) dibenzyl zinc + AA -> p2p (80-90%).

I read a thread of yours that seemed to indicate you couldn't make it work. Did you figure out what the problem was?

Although swim likes the look of the one-pot aldehyde/methylamine imine route to meth he thinks this is pretty interesting too.

No one seems to know whether the dibenzyl thing actually works.
Has anyone got refs on this?
Ideas for what the reaction mechanism of dibenzyl zinc + acetic anhydride is?

Related threads are:
82015
220932
107923
../rhodium/chemistry /phenylacetone.html
 
 
 
 
    Rhodium
(Chief Bee)
10-28-01 12:55
No 229560
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   


Ideas for what the reaction mechanism of dibenzyl zinc + acetic anhydride is?




Exactly the same as for a grignard reaction, just that the dibenzyl zinc is a less active reagent (the grignard rearranges to the wrong product if used).

 
 
 
 
    joyman
(Stranger)
10-28-01 17:58
No 229595
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

I think the first reaction is wrong it gives a grignard not dibenzyl zinc which is required in the second bit. (benzyl-Zn-Cl != (benzyl)2Zn)

Adding ZnCl2 to the grignard will give benzyl-Zn-Cl:
R-Mg-X + ZnCl2 --> R-Zn-Cl + MgXCl

ie Post No 104277
Blasie Ketone Synthesis: (from Organic Chemistry 6th Ed, 1957,  New York Booksellers) where treatment of a Grignard reagent with zinc chlorode gives an alkyl zinc Chloride
 
 
 
 
    joyman
(Stranger)
10-28-01 18:39
No 229601
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

but have also seen this

Post No 104156
2R-MgX + CdCl2 -> R-Cd-R + MgX2 + MgCl2
(ie the dibenzyl thing that we want)
 
 
 
 
    joyman
(Stranger)
10-30-01 18:33
No 230523
      Re: Forensics find an unusual meth synthesis in NZ  Bookmark   

allright i should have guessed, the answers already at rhodium's
deals with specificity of zinc and cadmium.
../rhodium/chemistry /grignard.notes.html