Boron tribromide → 5-Chloro-2-hydroxybenzene-1-sulfonamide
반응식
[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]=1참가 물질
4
반응 조건
- 온도
- -78 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-b01bc6866af44416bdc86c9e87868d5a
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07098212B2
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