HRID1868325
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A mixture of 7-bromo-2-phenyl-5H-thieno[3,2-c]pyridin-4-one 3 (2.28 g, 7.5 mmol) in phosphorus oxychloride (27 mL) was heated at reflux for 21 h. The reaction mixture was basified to pH 5-6 by the addition of saturated aqueous sodium carbonate and extracted with dichloromethane (1×). The organic layer was dried over Na2SO4, filtered, and the filtrate was purified by silica gel column chromatography (eluent: hexane:EtOAc, 97:3) to give 95.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 21 h
- extractionextracted with dichloromethane (1×)
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- customthe filtrate was purified by silica gel column chromatography (eluent: hexane:EtOAc, 97:3)