반응 #43322

반응 방정식

Potassium carbonate

sodium chlorodifluoroacetate

DMF

2-bromo-5-hydroxypyridine

→

title compound

수율 43.0%

2-bromo-5-difluoromethoxypyridine

수율 43.0%

용매

ether

반응 조건

후처리

1. 1
   기타The reaction liquid
2. 2
   온도was cooled to room temperature
3. 3
   세척washed with water
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축Concentrating the solvent under reduced pressure
6. 6
   기타the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

실험 절차

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%).

출처