반응 #43323

반응 방정식

DMF

ethanol

2-bromo-5-difluoromethoxypyridine

triethylamine

→

title compound

수율 80.0%

2-ethoxycarbonyl-5-difluoromethoxypyridine

수율 80.0%

용매

carbon monoxide

반응 조건

후처리

1. 1
   기타The reaction liquid
2. 2
   농축the solvent was concentrated under reduced pressure
3. 3
   workup.ADDITIONEthyl acetate was added to the resulting residue
4. 4
   세척by washing with water
5. 5
   건조drying over anhydrous magnesium sulfate
6. 6
   농축Concentrating the solvent under reduced pressure
7. 7
   기타the residue was purified on silica gel column chromatography (C-300, hexane:ethyl acetate=4:1-3:2)

실험 절차

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%).

출처