Ammonia → HCID 15811499, compound

Participants

Reaction Steps

260 ml. of concentrated ammonia solution were treated under an atmosphere of argon, and while cooling by means of ice/methanol bath at ≤-10° C. within about 20 minutes, with 164.5 g. of carbon disulfide and the mixture was subsequently stirred for an additional 15 minutes at the same temperature. 245 G. of 4-chlorobenzylamine dissolved in 122 ml. of acetonitrile were then slowly added, the temperature still maintained at ≤-10° C. Subsequently, the mixture was stirred overnight at room temperature and then cooled in an ice-bath to 0° C. The precipitated crystals were removed by filtration under suction, washed successively with acetonitrile and diethyl ether and dried to a constant weight under reduced pressure at 70°-80° C., and 390 g. of ammonium (N-4-chlorobenzyl)dithiocarbamate having a melting point of 140°-142° C. was obtained.

Provenance & Evidence