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A solution of 45,7 g (0.38 mole) of freshly distilled (Note 1) phenylacetaldehyde in 100 ml benzene was cooled to 0°C and a solution of 15.5 g (0.5 mole) of anhydrous methylamine in benzene (Note 2) was added.An exothermic reaction occured with separation of water; start refluxing with a Dean-Stark trap attached to the reflux condenser to collect the water that is generated in the reaction.When no more water separates, distill off the solvent and distill the aldimine.
Methyl Grignard reagent is prepared by adding 71 g (0.5 mole) of methyl iodide to a suspension of 12.2 g (0.5 mole) of Mg turnings in 150 ml dry ether.Adding a crystal of iodine speeds up the reaction.After about 1/2 hour standing, cool the Grignard reagent to 0°C and add dropwise the aldimine obtained in the previous step (this better be ~0.32 mole!) dissolved in the minimum amount of dry ether.After the addition, remove the ice-bath and start refluxing the solution (I guess for about 2 hours).Afterwards, decompose

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