反应详情

Hydrogen chloride was bubbled through a solution of 3-chlorobenzonitrile (25.5 g, 0.185 mol) in ethanol (250 mL) to saturation under ice-cooling and the reaction mixture was stirred at room temperature for 17 hours. The solvent was distilled off under reduced pressure and the residual solid was suspended in diethyl ether (200 mL), then collected by filtration, washed with diethyl ether (200 mL) and dried in vacuo at 60° C. to give 38.3 g (94%) of ethyl 3-chlorobenzimidate hydrochloride as white crystals.

1. temperaturecooling
2. distillationThe solvent was distilled off under reduced pressure
3. filtrationcollected by filtration
4. washwashed with diethyl ether (200 mL)
5. customdried in vacuo at 60° C.