HRID1868325

反应详情

EQUATION

反应方程式

HRID 1868325 反应方程式

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

  1. temperaturewas heated
  2. temperatureat reflux for 21 h
  3. extractionextracted with dichloromethane (1×)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customthe filtrate was purified by silica gel column chromatography (eluent: hexane:EtOAc, 97:3)