반응 #93541

반응 방정식

sodium hydrosulfide

α-methanesulfonyloxymethyl-β-phenyl-γ-butyrolactone

β-(p-chlorophenyl)-α-methanesulfonyloxymethyl-γ-butyrolactone

acetic acid

→

title compound

수율 52.0%

α-mercaptomethyl-β-phenyl-γ-butyrolactone

수율 52.0%

용매

ethyl acetate

ethanol

반응 조건

후처리

1. 1
   기타After completion of the reaction
2. 2
   세척washed with water in a conventional manner
3. 3
   건조dried over magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   기타The crude product thus obtained
6. 6
   기타was purified by a column chromatography

실험 절차

To a solution of 1.0 g of α-methanesulfonyloxymethyl-β-phenyl-γ-butyrolactone (III) in 20 ml of ethanol were added 1.5 ml of acetic acid and then 1.2 g of commercially available 70% sodium hydrosulfide and the mixture was stirred at room temperature for 18 hours. After completion of the reaction, the reaction mixture was diluted with 150 ml of ethyl acetate, washed with water in a conventional manner, dried over magnesium sulfate and the solvent was distilled off. The crude product thus obtained was purified by a column chromatography to give 400 mg (yield 52%) of the title compound.

출처