반응 #158353

반응 방정식

ethyl 2-oxopiperidine-3-carboxylate

sulfuryl chloride

sodium hydrogen carbonate

→

title compound

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

용매

THF

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 30 min
2. 2
   추출extracted with ethyl acetate (300 mL×3)
3. 3
   세척The extract was washed with saturated brine (300 mL)
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타the solvent was evaporated under reduced pressure
6. 6
   세척The residue was washed with hexane/ethyl acetate (5/1, 60 mL×2)

실험 절차

To a mixture of ethyl 2-oxopiperidine-3-carboxylate (30 g) in THF (300 mL) was added dropwise sulfuryl chloride (14.2 mL) at 0° C.-5° C., and the mixture was stirred at room temperature for 18 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution (300 mL) at 0° C., and the mixture was stirred at room temperature for 30 min and extracted with ethyl acetate (300 mL×3). The extract was washed with saturated brine (300 mL), and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was washed with hexane/ethyl acetate (5/1, 60 mL×2) to give the title compound (32.7 g). MS (ESI+): [M+H]+ 206.1.

출처