HRID1595478
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
CONDITIONS
反应条件
- 温度
- 210 °C
PROCEDURE
实验过程
3.9 g (11 mmole) 5-(4-[2-(4-cyanophenyl)ethoxy]benzylidene)thiazolidine-2,4-dione and 3.88 g (15 mmole) diethyl-1,4-dihydro-2,6-dimethyl-3,5-pyridine dicarboxylate were mixed and heated to 210° C. under vacuum for 1 hour. The solid material was dissolved in ethyl acetate, evaporated in vacuo, purified by chromatography on silica gel with first dichloromethane, then dichloromethane:diethyl ether (95:5) and finally dichloromethane:methanol (95:5) as eluents. Crystallization in acetone/water gave 0.65 g (yield 17%) of the desired product.
WORKUP
后处理
- customevaporated in vacuo
- custompurified by chromatography on silica gel with first dichloromethane
- customCrystallization in acetone/water