Chloroform → 4-Methanesulfinylaniline
反応式
[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]参加物
5
反応条件
- 温度
- 0 °C
実験手順
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%).
後処理
- washIt was then washed with saturated NaHCO3 solution
- dry with materialdried over MgSO4
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-e8a8d2ac77b541d88a8e0b11e1abec61
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06743816B2
反応ノート
読み込み中…