反应 #43323

反应方程式

DMF

ethanol

2-bromo-5-difluoromethoxypyridine

triethylamine

→

title compound

收率 80.0%

2-ethoxycarbonyl-5-difluoromethoxypyridine

收率 80.0%

溶剂

carbon monoxide

反应条件

后处理

1. 1
   其他The reaction liquid
2. 2
   浓缩the solvent was concentrated under reduced pressure
3. 3
   workup.ADDITIONEthyl acetate was added to the resulting residue
4. 4
   洗涤by washing with water
5. 5
   干燥drying over anhydrous magnesium sulfate
6. 6
   浓缩Concentrating the solvent under reduced pressure
7. 7
   其他the residue was purified on silica gel column chromatography (C-300, hexane:ethyl acetate=4:1-3:2)

实验过程

A DMF (15 mL)-ethanol (15 mL) mixed solvent solution of 2-bromo-5-difluoromethoxypyridine (1.32 g, 5.89 mmols), palladium acetate (132 mg, 0.59 mmol), 1,1′-bis(diphenylphosphino)ferrocene (654 mg, 1.18 mmols) and triethylamine (1.6 mL, 11.8 mmols) was stirred overnight at 50° C. in carbon monoxide atmosphere. The reaction liquid was cooled to room temperature and the solvent was concentrated under reduced pressure. Ethyl acetate was added to the resulting residue, followed by washing with water and drying over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was purified on silica gel column chromatography (C-300, hexane:ethyl acetate=4:1-3:2) to provide the title compound (1.03 g, 80%).

来源