反応 #93541

反応方程式

sodium hydrosulfide

α-methanesulfonyloxymethyl-β-phenyl-γ-butyrolactone

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

acetic acid

→

title compound

収率 52.0%

α-mercaptomethyl-β-phenyl-γ-butyrolactone

収率 52.0%

溶媒

ethyl acetate

ethanol

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   洗浄washed with water in a conventional manner
3. 3
   乾燥dried over magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   その他The crude product thus obtained
6. 6
   その他was purified by a column chromatography

実験手順

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.

出典