Boron tribromide → 5-Chloro-2-hydroxybenzene-1-sulfonamide
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:12]C)=[C:6]([S:8]([NH2:11])(=[O:10])=[O:9])[CH:7]=1.B(Br)(Br)Br>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:12])=[C:6]([S:8]([NH2:11])(=[O:10])=[O:9])[CH:7]=1参加物
4
反応条件
- 温度
- -78 °C
実験手順
To a suspension of 5-chloro-2-methoxy-benzenesulfonamide (0.52 g, 2.33 mmol) in dichloromethane (25 mL) at −78° C. was added boron tribromide (1M solution in dichloromethane, 3.5 mL, 3.5 mmol). The reaction was stirred at −78° C. for 30 minutes and then warmed to ambient temperature and stirred overnight. The reaction was quenched with water (0.30 mL) and the precipitate formed was removed by filtration. The filtrate was concentrated in vacuo and the crude product was purified by chromatography on silica gel to give the title compound (0.32 g).
後処理
- temperaturewarmed to ambient temperature
- stirringstirred overnight
- customThe reaction was quenched with water (0.30 mL)
- customthe precipitate formed
- customwas removed by filtration
- concentrationThe filtrate was concentrated in vacuo
- customthe crude product was purified by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-b01bc6866af44416bdc86c9e87868d5a
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098212B2
反応ノート
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