반응 #158291

반응 방정식

ammonium chloride

sodium ethoxide

diethyl (3,4-difluorophenyl)propanedioate

Acrylonitrile

→

title compound

diethyl (2-cyanoethyl)(3,4-difluorophenyl)propanedioate

용매

tert-butylalcohol

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature overnight
2. 2
   추출the mixture was extracted with ethyl acetate
3. 3
   세척The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타The solvent was evaporated under reduced pressure

실험 절차

Under an argon atmosphere, sodium ethoxide (20% ethanol solution, 1.7 g) was added to a mixture of diethyl (3,4-difluorophenyl)propanedioate (13.8 g) in tert-butylalcohol (50 mL) at room temperature, and the mixture was stirred at 40° C. for 30 min. Acrylonitrile (3.34 mL) was added to the reaction mixture at room temperature, and the mixture was stirred at room temperature overnight. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (15.2 g).

출처