Water → 4-Benzhydrylpiperazin-1-yl carbonyl chloride

Participants

Reaction Steps

A solution of 2.522 g (10 mmol) of 1-benzhydrylpiperazine and of 1.62 ml (20 mmol) of pyridine in 15 ml of dichloromethane is added, dropwise, to a solution of 1.187 g (4 mmol) of triphosgene in 10 ml of dichloromethane, cooled to −5° C. under an argon atmosphere. Stirring is continued at −5° C. for 15 minutes and then at ambient temperature for 3 hours. 50 ml of dichloromethane and 50 ml of water are subsequently added. The mixture is separated by settling out and the organic phase is washed with 2×25 ml of water and then 25 ml of a saturated aqueous solution of sodium chloride. The product is dried over sodium sulfate and evaporated under vacuum, so as to obtain 2.72 g of product in the form of a gum, used as it is in the following step.

Provenance & Evidence