反应 #43322

反应方程式

Potassium carbonate

sodium chlorodifluoroacetate

DMF

2-bromo-5-hydroxypyridine

→

title compound

收率 43.0%

2-bromo-5-difluoromethoxypyridine

收率 43.0%

溶剂

ether

反应条件

后处理

1. 1
   其他The reaction liquid
2. 2
   温度was cooled to room temperature
3. 3
   洗涤washed with water
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   浓缩Concentrating the solvent under reduced pressure
6. 6
   其他the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

实验过程

Potassium carbonate (2.4 g, 17.3 mmols) and sodium chlorodifluoroacetate (4.2 g, 27.5 mmols) were added to a DMF (20 mL) solution of 2-bromo-5-hydroxypyridine (2.4 g, 13.8 mmols) and stirred overnight at 80° C. The reaction liquid was cooled to room temperature, added ether, washed with water and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2) to provide the title compound (1.32 g, 43%).

来源