反応式
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]参加物
6
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.
後処理
- customAfter completion of the reaction
- washwashed with water in a conventional manner
- dry with materialdried over magnesium sulfate
- distillationthe solvent was distilled off
- customThe crude product thus obtained
- customwas purified by a column chromatography
出典と根拠
- ORDレコード
- ord-62844afc2adb4bd9bea5546d1bc4665b
- 出典データセット
- uspto-grants-1986_09
- 特許番号
- US04613613
関連ノート
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