반응 #158290

반응 방정식

ammonium chloride

sodium hydride

diethyl carbonate

ethyl (3,4-difluorophenyl)acetate

→

title compound

diethyl (3,4-difluorophenyl)propanedioate

용매

THF

THF

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux for 2 hr
3. 3
   추출the mixture was extracted with ethyl acetate
4. 4
   세척The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   기타the solvent was evaporated under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

A mixture of ethyl (3,4-difluorophenyl)acetate (11.3 g) in THF (50 mL) was added to a mixture of sodium hydride (60%, 4.74 g), diethyl carbonate (34.2 mL) and THF (250 mL) at room temperature, and the mixture was heated under reflux for 2 hr. 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, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (13.8 g).

출처