反应 #73904

反应方程式

5-Bromobenzofuran-2-carboxylic acid

sodium bicarbonate

Selectflor

→

5-Bromo-2-fluoro-1-benzofuran

溶剂

carbon tetrachloride

dichloromethane

sodium hydroxide

water

反应条件

后处理

1. 1
   其他The organic phase was separated
2. 2
   洗涤washed with brine
3. 3
   干燥dried over anhydrous MgSO4
4. 4
   其他The solvent was evaporated under reduced pressure at room temperature
5. 5
   洗涤eluted with diethyl ether

实验过程

5-Bromobenzofuran-2-carboxylic acid (4.68 g) was suspended in carbon tetrachloride (150 ml) and water (50 ml). To this was added sodium bicarbonate (3.36 g), followed by Selectflor (7.1 g) and the reaction mixture was stirred rapidly for 20 hours. The reaction mixture was diluted with dichloromethane and 2N sodium hydroxide solution. The organic phase was separated, washed with brine and dried over anhydrous MgSO4. The solvent was evaporated under reduced pressure at room temperature. The residue was applied to a silica cartridge (20 g) and eluted with diethyl ether. This gave 5-bromo-2-fluoro-1-benzofuran (1.4 g).

来源