1b) (alternative) JACS 70, 3868 (1948)
Distill methylamine gas (prepared by dripping 50% NaOH in water over methylamine hydrochloride crystals) onto cooled phenylacetaldehyde (45.7 g, 0.38 mole) while stirring until the solution has gained about 15 g (0.5 mole) of methylamine. Let stand for 1-2 hrs under cooling and stirring. Extract the mixture with dry ether, dry the ether and evaporate the solvent to get about 80-90% yield of aldimine. With the aldimine in hand, it's important to proceed directly to the next step: the preparation of a methyl Grignard solution in ether.
Well, this suggests that you can just bubble some MeAm gas through phenylacetaldehyde without solvent, so then this can be done at RT, cool in ice bath with stirring and then extract with solvent, hopefully something other than ether.
I am assuming the P2P has a short shelf life since this says the aldimine should be used directly after making it.
I can't beleive I overlooked that part, does any one have any advice with this?
Game Plan
Treat an aqueous solution of 20g of l-phenylalanine in 500ml water with an aqueous 0.3N solution of sodium hypochlorite in 300ml water. I am shady on this part since this is where SWIM is suposed to solvent extract the aqueous layer. Anyway, take the resulting aldehyde and hook up to a gassing advice, take freshly prepared methylamine and create the gas with a solution of NaOH, probably an eye dropper, beer bottle, tubing, and rubber stopper will be used to gas, all the while measuring on a gram scale to make sure the solution gains 5g and then cool with stirring and proceed to reduction of choice, how does this sound, incomprehensible, unrealistic, shady, input please.
