反应详情

Triethylamine (260 mg) was added to a solution of 1-{[4-ethoxycarbonylamino-1-(2-methyl-4-pyridyl)-4-piperidinyl]methyl}-2-piperazinone hydrochloride (263 mg) in dichloromethane (20 ml), 4-vinylbenzenesulfonyl chloride (194 mg) was added at 0° C., and the mixture was stirred at room temperature for 1 hour. To the reaction solution was added an aqueous sodium carbonate solution, the material was extracted with dichloromethane, dried, concentrated, purified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1), and crystallized from diisopropyl ether to obtain the colorless crystalline title compound (157 mg).

1. additionwas added at 0° C.
2. extractionthe material was extracted with dichloromethane
3. customdried
4. concentrationconcentrated
5. custompurified by column chromatography (dichloromethane:10% aqueous ammonia-containing methanol=20:1)
6. customcrystallized from diisopropyl ether