Acetic Acid → alpha-Mercaptomethyl-beta-phenyl-gamma-butyrolactone

HRID 65263

반응식

HRID 65263 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][O:12][C:10](=[O:11])[CH:9]2[CH2:14]OS(C)(=O)=O)=[CH:4][CH:3]=1.C(O)(=O)C.[SH-:24].[Na+]>C(O)C.C(OCC)(=O)C>[SH:24][CH2:14][CH:9]1[CH:8]([C:5]2[CH:4]=[CH:3][CH:2]=[CH:7][CH:6]=2)[CH2:13][O:12][C:10]1=[O:11]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 28015Sodium hydrosulfideHCID 13518915beta-(p-Chlorophenyl)-alpha-methanesulfonyloxymethyl-gamma-butyrolactone

생성물 1

HCID 13518975alpha-Mercaptomethyl-beta-phenyl-gamma-butyrolactone수율 52%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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.

후처리

  1. customAfter completion of the reaction
  2. washwashed with water in a conventional manner
  3. dry with materialdried over magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customThe crude product thus obtained
  6. customwas purified by a column chromatography

출처 및 근거

ORD 기록
ord-62844afc2adb4bd9bea5546d1bc4665b
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613613

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