반응 #158354

반응 방정식

3,4,5-trifluorophenol

potassium carbonate

water

ethyl 3-chloro-2-oxopiperidine-3-carboxylate

→

title compound

수율 79.8%

ethyl 2-oxo-3-(3,4,5-trifluorophenoxy)piperidine-3-carboxylate

수율 79.8%

용매

DMF

brine

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The extract was washed with saturated aqueous sodium hydrogen carbonate solution (200 mL), water (200 mL) and saturated brine (200 mL×2)
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타the solvent was evaporated under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

To a mixture of 3,4,5-trifluorophenol (14.4 g) and potassium carbonate (40.3 g) in DMF (200 mL) was added ethyl 3-chloro-2-oxopiperidine-3-carboxylate (20 g), and the mixture was stirred at 100° C. for 1 hr. To the reaction mixture were added water (200 mL) and saturated brine (200 mL) at 0° C., and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution (200 mL), water (200 mL) and saturated brine (200 mL×2), and dried over anhydrous magnesium 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 (24.61 g).

출처