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Topic: P2P or amph. from benzyl magnesium chloride and acetonitrile grignard reaction (Read 732 times)
lugh
Global Moderator
Foundress Queen
Posts: 876
Re: P2P or amph. from benzyl magnesium chloride and acetonitrile grignard reaction
« Reply #20 on: July 04, 2010, 02:31:28 PM »
A bisulfite adduct wouldn't form using the organic product from the reaction of benzylmagnesium chloride and acetonitrile using the procedure from JOC51 5338-41 (1986) & 52 3901-4 (1987)
Chemistry is our Covalent Bond
Evilblaze
Guest
Re: P2P or amph. from benzyl magnesium chloride and acetonitrile grignard reaction
« Reply #21 on: January 11, 2011, 12:45:54 AM »
Another run was made.
250g benzl-chloride 99% pure 60g magnesium shavings 99% pure 500ml diethyl ether 99,6% pure 130g acetonitile 99,8% pure yield 108g P2P, nearly 50% yield +95% pure, boiling point, denstity ok.
The grignard reagent and the acetonitrile.
The formed intermedier after the addition of the acetonitrile.
The yielded ethereal solution with P2P in it.
Electro´S
Pupae
Posts: 95
Re: P2P or amph. from benzyl magnesium chloride and acetonitrile grignard
« Reply #22 on: January 03, 2013, 10:49:19 AM »
After getting lost with "metal/acid nitroreductions" was investigated "the legendary classic route" to amphetamine via grignard from Benzyl chloride (or cyanide) and acetonitrile with NaBH4. The yields for the ketone are not good enough but some one said high yields in the amine formation. Practically is needed a flame or microwave to dry the glassware, molecular sieves to dry the ether, and a ultrasonic bath to kick start the reaction of the grignard reagent. A good condensor is recomended to keep the solvent inside the flask and inert gas or a calcium chloride tube to keep out moisture in the reaction. After addition of acetonitrile, is commented a white precipitate is formed. and it can be isolated by filtration or reduced with NaBH4 in a "one pot synth".
On the paper sounds great!!! Not impossibles reagents like nitroethane, with a ultrasonic bath in the Rodhium´s archives succes in grignard reaction are obtained even with not dry-ether and wet weather, and the possibility of one pot way from precursor to final product make of this reaction a powerfull tool to keep in mind.
And finally some one (I can´t find where i read it) propose one method to form the "Piperonyl-Magnesium" reagent from piperonil chloride.
if Any one had experience or recomendations on this routes, is welcome. I prefer ask here before open a new thread wich would end in nothing
I like grignard!!!
« Last Edit: January 04, 2013, 11:00:51 PM by lugh »