by Benzylmagnesium Chloride Alkylation of Acetaldehyde Methylimine
by Leno Latrunculus
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Well, I think I got it all together, since no-one seems to have done this not-me thinks he will boldly go where no bee has gone before. This will be done on the following scale: 2.025g Mg covered in 8.325ml. ether, the stirrer will be started and 3.125ml. of a mixture of 10.5375ml. benzyl chloride dissolved in 41.663ml. ether will be dripped in and left for 30 min. until the reaction starts. The remainder will be dripped in over a 30 min. period. The reaction temp. will be kept as close to 45°C as possible by immersion in an ice bath. After the reaction has subsided it will be refluxed for 15-30 min. on non-explosion proof hotplate. Immediately following 5.5g of methylamine HCl and 5.5g of acetaldehyde dissolved in 61ml of ether chilled to 0°C will be slowly added dropwise over 30 min. After the reaction has stopped the temp. will be allowed to rise to approx. 50°C and will be refluxed for 1-1.5 hrs the temp will again be allowed to rise to approx 55-60°C and distilled for approx. 2.5-3hrs. to ensure all the solvent has been distilled off. After this has ended 25ml. of ether in 100ml of 10% HCl will be poured into the flask. The ether will be distilled off and 25% NaOH will be added to the flask until a pH of 10 is reached. The contents of the flask will be poured into a 250ml. sep. funnel and extracted with 2x25 ml. portions of DCM.
The extracts will be combined in a 250ml. flask and saturated with dry HCl generated from dripping HCl onto non iodinized salt, the gas will pass thru a dreschel bottle fitted with a med. bubbler and containing sulfuric acid and will pass into the 250ml. flask containing the extracts. The precipitate will be recrystallized from dry 2-propanol and xylene.
I will check back once more in hope someone has any additional info. for me, if not I will let you know how it went for not-me. If anyone is really knowledgable please check this thread often as not-me may run into some problems and need some helpful advice.
Then help me out with some tests to perform, as I stated I am not in a position to perform proper tests until next week. I am anxious too, maybe you are aware of a simple test such as solubility etc. I already performed a m.p. test and it was 1.6°C higher than it should be. I don't know if that makes a big difference as this wasn't exactly done by A.C.S standards.
Oh baby, just finished my tests and came up with mp. 172°C, and the IR spectrum was the same that was stated and reported for the substance. Gave a close aquantance a sample and they refered to not-me as a god-like nirvanic figure. This shit works, thanks yy4uguys and I found out why the yields were low, MY FUCKUP, did it again and got a 82% molar yield, FUCK YAH, this shit kicks the HI/RP methods ass. I wll post my screw-ups so you all don't repeat the same shit. Oh yah, for all that care I forgave the cat, fuck I luv the cat, all is forgiven. Old monsier(sp?) Victor Grignard is one cool cat.