تفاعل #43323

معادلة التفاعل

DMF

ethanol

2-bromo-5-difluoromethoxypyridine

triethylamine

→

title compound

المردود 80.0%

2-ethoxycarbonyl-5-difluoromethoxypyridine

المردود 80.0%

المذيبات

carbon monoxide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   تركيزthe solvent was concentrated under reduced pressure
3. 3
   workup.ADDITIONEthyl acetate was added to the resulting residue
4. 4
   غسيلby washing with water
5. 5
   تجفيفdrying over anhydrous magnesium sulfate
6. 6
   تركيزConcentrating the solvent under reduced pressure
7. 7
   أخرىthe residue was purified on silica gel column chromatography (C-300, hexane:ethyl acetate=4:1-3:2)

الإجراء التجريبي

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%).

المصدر