To me this looks better than Lenos work.
Improvements in the manufacture of organic compounds containing nitrogen, arsenic, sulphur or selenium
EXAMPLE 1 44 gms. of acetaldehyde are dropped slowly, with constant stirring, into 100 gms of benzyl-magnesium chloride dissolved in 150 ccs. of absolute ether. The temperature rises slowly to 50 C. which is kept constant for two hours. The magnesium alkoxide obtained, having the formula C6H3.CH2.CH(OMgCl)CH3, is treated for three hours with gaseous methyl-amine. The reaction product, which becomes heated during the reaction, is allowed to cool slowly and is then extracted with ether and the ethereal solution is dried over magnesium sulphate. The ether is then carefully removed, pervitin, corresponding to the formula EMI3.1 being obtained as residue.
http://v3.espacenet.com/publicationDetails/description?CC=GB&NR=782887A&KC=A&FT=D&date=19570911&DB=EPODOC&locale=en_GBExperimental:
Preparation of benzylmagnesium chloride:
In a flask equipped with an addition funnel and a cooling bath, benzylmagnesium chloride was prepared by dripping 24.4g (0.2 mol) of freshly distilled benzyl chloride (bp 179°C) dissolved in ether in small portions onto 4.8 gram (0.2 mol) of cleaned magnesium turnings covered with ether. The initiation of the reaction can be facilitated by heating the magnesium turnings in a test-tube with an iodine crystal before use. After the addition of all the reagent, the solution was boiled until all the magnesium was dissolved.
Preparation of etheral methylamine:
In a fractional distilling apparatus there was introduced 15g of methylamine hydrochloride, and from an addition funnel, there was slowly added 30ml of a 40% sodium hydroxide solution. The evolved methylamine gas was lead into an ice-cooled flask filled with anhydrous ether and some anhydrous sodium sulfate. To prevent the escape of gas and enrance of moisture, the recieving flask was connected to a U-tube filled with mercury. A 5ml portion of the etheral solution of methylamine was poured into a little water and quickly titrated in the presence of methyl orange with a standardized acid solution to determine the concentration of methylamine.
Preparation of acetaldehyde:
The acetaldehyde was prepared immediately before use by the depolymerization of paraldehyde. In an apparatus similar to that for the production of methylamine, concentrated sulfuric acid was added to paraldehyde, which distilled at a temperature of 21°C into a reciever cooled in ice.
Preparation of the imine and reaction with the grignard reagent:
A cold solution of etheral methylamine, containing 3.1g of the free base (0.1 mol) was mixed with a cooled etheral solution of 4.4g of acetaldehyde, whereupon the solution became turbid. Anhydrous sodium sulfate was added with swirling of the mixture to absorb the formed water, and the solution was decanted into the addition funnel of the flask containing the pre-made benzylmagnesium chloride, which in the meantime had been cooled in an ice-bath, and was added dropwise to the solution.
After it had all reacted the solution was acidified and washed with ether to remove by-products, basified with a sodium hydroxide solution and extracted repratedly with ether, the ether extracts dried over anhydrous sodium sulfate, filtered and concentrated to give an oil, which was neutralized by the addition of concentrated hydrochloric acid giving a wet, crystalline mass that was dried for several days in a desiccator containing both concentrated sulfuric acid and solid sodium hydroxide. The obtained crystals was recrystallized repeatedly from acetone to give colorless crystals of methamphetamine hydrochloride with a melting point of ca 140°C, in ca 40% yield.
Sorry for cut/paste. Couldnt post the original link as it seems to be broke.
