Chloroform → 4-Methanesulfinylaniline
반응식
[CH3:1][S:2][C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1.ClC1C=CC=C(C(OO)=[O:18])C=1.C(Cl)(Cl)Cl>C(Cl)Cl>[CH3:1][S:2]([C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1)=[O:18]참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
20 g (143.66 mmol) of 4-methylthioaniline was placed in a flask and dissolved in 660 mL of CH2Cl2. The solution was cooled to 0° C. and 35.42 g (143.66 mmol) of m-chloroperbenzoic acid was added. The mixture was stirred for 3 h at room temperature and poured into CHCl3. It was then washed with saturated NaHCO3 solution, dried over MgSO4 and the solvent was removed, yielding a crude product that was purified by chromatography on silica gel, using MeOH/EtOAc/hexane mixtures of increasing polarity as eluent. The title compound of the example was obtained as a white solid (17.84 g, 80%).
후처리
- washIt was then washed with saturated NaHCO3 solution
- dry with materialdried over MgSO4
- customthe solvent was removed
출처 및 근거
- ORD 기록
- ord-e8a8d2ac77b541d88a8e0b11e1abec61
- 출처 데이터셋
- uspto-grants-2004_06
- 특허 번호
- US06743816B2
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