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