反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
6-[4-(3,4-Dimethoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril (1.96 g) and 0.25 g of 50% oily sodium hydride were mixed with 60 ml of DMF and stirred at room temperature for 2 hours. Then, to the mixture was added 0.66 g of propargyl chloride and the mixture was stirred at room temperature for 7 hours. The reaction mixture was poured into a 150 ml of saturated saline solution and organic substances were extracted with chloroform. The chloroform layer was washed with water and dehydrated. Chloroform was distilled off and the residue was purified through silica gel column chromatography followed by recrystallization from ethanol to give 0.34 g of 1-(2-propynyl)-6-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril, m.p. 152°-154° C., pale yellow needles.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 7 hours
- extractionwere extracted with chloroform
- washThe chloroform layer was washed with water
- distillationChloroform was distilled off
- customthe residue was purified through silica gel column chromatography
- customfollowed by recrystallization from ethanol