Chlorosulfonic acid → 2-Bromo-4,5-dimethoxybenzene-1-sulfonyl chloride
反応式
[Br:1][C:2]1[CH:3]=[C:4]([O:10][CH3:11])[C:5]([O:8][CH3:9])=[CH:6][CH:7]=1.[Cl:12][S:13](O)(=[O:15])=[O:14]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([O:10][CH3:11])[C:5]([O:8][CH3:9])=[CH:6][C:7]=1[S:13]([Cl:12])(=[O:15])=[O:14]参加物
4
実験手順
To a cooled (0° C.) solution of 4-bromoveratrole (15 mL, 100 mmol) in dichloromethane (100 mL) was added dropwise chlorosufonic acid (26 mL, 400 mmol). The reaction was allowed to slowly warm to ambient temperature and maintained for 3 hours, at which time it was concentrated and diluted with ether (300 mL). The resultant solution was then washed with ice cold water (2×250 mL) and brine (100 mL), dried over magnesium sulfate, and concentrated to furnish a grayish powder (25 g, 78%).
後処理
- temperaturemaintained for 3 hours, at which time it
- concentrationwas concentrated
- additiondiluted with ether (300 mL)
- washThe resultant solution was then washed with ice cold water (2×250 mL) and brine (100 mL)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-46af6e94c9c24c6281c66808f94be677
- 出典データセット
- uspto-grants-2006_04
- 特許番号
- US07026349B2
反応ノート
読み込み中…