反応 #43322

反応方程式

Potassium carbonate

sodium chlorodifluoroacetate

DMF

2-bromo-5-hydroxypyridine

→

title compound

収率 43.0%

2-bromo-5-difluoromethoxypyridine

収率 43.0%

溶媒

ether

反応条件

後処理

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

実験手順

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%).

出典