Methylamine → 2-Hydroxyphenyl methylsulfamate
反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[O:3][S:2]1(=[O:11])=[O:10].[CH3:12][NH2:13]>C1COCC1.C(OCC)(=O)C>[CH3:12][NH:13][S:2](=[O:11])(=[O:10])[O:1][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[OH:3]参加物
5
実験手順
To a solution of 1,3,2-benzodioxathiol 2,2-dioxide (300 mg) in THF (6 mL) was added methylamine (0.871 mL, 2 M THF solution) at room temperature, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was diluted with ethyl acetate. The diluted solution was washed with distilled water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (86 mg).
後処理
- washThe diluted solution was washed with distilled water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel chromatography (hexane/ethyl acetate)
出典と根拠
- ORDレコード
- ord-fec88b87266840f0870fc48372b7a6b2
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722662B2
反応ノート
読み込み中…