反应 #2507830

反应方程式

water

triphenylphosphine

bromine

(6-fluoro-3-pentylchroman-7-yl)methanol

→

7-bromomethyl-6-fluoro-3-pentylchroman

溶剂

acetonitrile

acetonitrile

反应条件

后处理

1. 1
   萃取the mixture is extracted three times with n-heptane
2. 2
   洗涤phases are washed with water
3. 3
   干燥dried over sodium sulfate
4. 4
   其他The solvent is removed in vacuo
5. 5
   过滤the residue is filtered through silica gel with heptane/toluene (4:1)

实验过程

10.2 g (38.9 mmol) of triphenylphosphine are suspended in 80 ml of acetonitrile, and 2.0 ml (39.0 mmol) of bromine are added dropwise with ice cooling. A solution of 10.0 g (38.4 mmol) of (6-fluoro-3-pentylchroman-7-yl)methanol in 20 ml of acetonitrile is subsequently added, and the mixture is stirred overnight at room temp. After addition of water, the mixture is extracted three times with n-heptane, and the combined org. phases are washed with water and dried over sodium sulfate. The solvent is removed in vacuo, and the residue is filtered through silica gel with heptane/toluene (4:1), giving 7-bromomethyl-6-fluoro-3-pentylchroman as a colourless oil.

来源