4-Fluorobenzoyl chloride → Phenylmethyl 4-[(4-fluorobenzoyl)amino]-1-piperazinecarboxylate

Participants

Reaction Steps

Crude 1-amino-4-benzyloxycarbonylpiperazine (433 g) and triethylamine (254 ml) were dissolved in dry methylene chloride(1.81) and to this solution was added dropwise p-fluorobenzoyl chloride (225 g) under cooling in an ice-bath at 8~25° C. for a period of 20 minutes. The reaction mixture was stirred for 1 hour at ambient temperature and then the resultant crystal was collected by filtration and washed with methylene chloride (300 ml), diisopropyl ether (500 ml) and water (1.51) successively to give N-(4-benzyloxycarbonyl-1-piperazinyl)-4-fluorobenzamide (327 g) as a white powder.

Provenance & Evidence