HRID70696

反应详情

EQUATION

反应方程式

HRID 70696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

48% hydrobromic acid (7 mL) was added to a solution of [3-chloro-4-(methylsulfanyl)phenyl](6-methoxy-5-methylpyridin-2-yl)methanone obtained in Reference Example 1-40 (700 mg) in acetonitrile (7 mL) at room temperature, and the mixture was stirred at 95° C. for one hour. The reaction solution was neutralized with saturated aqueous sodium bicarbonate at room temperature and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=50:1) to give 6-[3-chloro-4-(methylsulfanyl)benzoyl]-3-methylpyridin-2(1H)-one as a pale yellow solid (632 mg, 95%).

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customThe solvent was then evaporated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (chloroform:methanol=50:1)