Dichloroacetyl chloride → HCID 19826608, compound

Participants

Reaction Steps

A solution consisting of 23.8 g of N-(3,4-dimethoxybenzyl)-N-(2-methoxy-1-methylethyl)amine (prepared by condensing 3,4-dimethoxybenzylamine and methoxy acetone and hydrogenating the condensation product), 80 ml of toluene, and 20 ml of water in which 4 g of solid sodium hydroxide were dissolved is prepared and cooled down to -10° to -15°. Another solution of 14.7 g of dichloroacetylchloride in 10 ml of toluene is then added dropwise thereto while stirring. The mixture is stirred for one hour after all the dichloro-acetylchloride is added and the poured into 1 l of ice-water. The organic layer that formed was then extracted with ether, washed with diluted hydrochloric acid and twice with water, dried and concentrated. The residue crystallises spontaneously and yields 30.9 g of raw product melting at 62°-63°. After recrystalliation from a toluene/pentane mixture one obtained 21.3 g of pure title product melting at 75°-76°.

Provenance & Evidence