反应详情

1.2 g of 1-{4-[N-(2-isopropyloxyethyl)amino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine are dissolved in 15 ml of toluene, and 1.1 g of potash are added. The mixture is stirred for 10 minutes at RT and then 1.9 g of chloroformic acid benzyl ester in 4 ml of toluene are added dropwise thereto. The mixture is stirred overnight at RT and concentrated by evaporation, the residue is partitioned between dichloromethane and water, and the mixture is concentrated by evaporation and chromatographed over silica gel (eluant: dichloromethane/acetone 9:1). Treatment with alcoholic hydrochloric acid yields 1-{4-[N-(2-isopropyloxyethyl)benzyloxycarbonylamino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine hydrochloride having a melting point of 135°-137°.

1. stirringThe mixture is stirred overnight at RT
2. concentrationconcentrated by evaporation
3. customthe residue is partitioned between dichloromethane and water
4. concentrationthe mixture is concentrated by evaporation
5. customchromatographed over silica gel (eluant: dichloromethane/acetone 9:1)