Methanol → 5-Chloro-2-methylsulfonylindan-1-one
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[CH:6](SC)[CH2:5]2.[OH:14][S:15]([O-:18])(=O)=O.[K+].[CH3:20]O>O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[CH:6]([S:15]([CH3:20])(=[O:18])=[O:14])[CH2:5]2参加物
5
実験手順
0.5 g (2.35 mmol) of 5-chloro-2-methylsulfanylindan-1-one is dissolved in 10 ml of methanol; at 0° C., a solution of 4.33 g (7.05 mmol) of 2KHSO5×KHSO4×K2SO4 in 10 ml of water is added dropwise. The mixture is stirred at room temperature for 5 h; the methanol is distilled off and the aqueous residue is extracted with dichloromethane. The organic phase is separated off, dried over MgSO4, filtered and concentrated under reduced pressure. This gives 0.5 g of 5-chloro-2-methanesulfonylindan-1-one of melting point 197° C.
後処理
- distillationthe methanol is distilled off
- extractionthe aqueous residue is extracted with dichloromethane
- customThe organic phase is separated off
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-238b26a1f1c34f19adaee31e582da7c5
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06667345B2
反応ノート
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