Dichloromethane → 2-Bromophenylmethylsulfoxide
反応式
[OH:1]OS([O-])=O.[K+].[Br:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14][CH3:15].C(=O)(O)[O-].[Na+].ClCCl>O.CC(C)=O>[Br:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14]([CH3:15])=[O:1]参加物
7
実験手順
Oxone (9.7 g) in water (40 ml) was added slowly to a stirred, cooled cooled (0° C.) solution of 2-bromothioanisole (5 g, 24.6 mmol) and sodium bicarbonate (16 g) in acetone (20 ml). The mixture was stirred for at room temperature 16 h., then water and dichloromethane was added. The layers were separated and the organic phase was dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was purified by chromatography on silica gel, eluting with hexane/EtOAc (80:20 increasing to 40:60) to give the title compound (6.1 g). m/z (ES+) 219 (M+1).
後処理
- temperaturecooled
- customThe layers were separated
- dry with materialthe organic phase was dried (MgSO4)
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by chromatography on silica gel
- washeluting with hexane/EtOAc (80:20 increasing to 40:60)
出典と根拠
- ORDレコード
- ord-05da3fab12bc48b6b6030ec94b6d3426
- 出典データセット
- uspto-grants-2000_06
- 特許番号
- US06071927
反応ノート
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