Dimethylamine → 3-(N,N-dimethylsulfamoyl)benzoic acid
反応式
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].[CH3:14][NH:15][CH3:16].C1COCC1>C(Cl)Cl>[CH3:14][N:15]([CH3:16])[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3]参加物
5
実験手順
A solution of 3-(chlorosulfonyl)benzoic acid (152 mg, 0.689 mmol) in methylene chloride (2 mL) was treated with 2.0 M dimethylamine in THF (1.137 mL, 2.274 mmol), and the mixture was stirred overnight at room temperature. The reaction was quenched with 1 N HCl, and extracted 3× with EtOAc. The combined organic phases were washed with 1 N HCl followed by brine, then dried over sodium sulfate and concentrated in-vacuo to yield the title compound (138 mg, 0.602 mmol, 87% yield). MS (ESI+)=230.18, (M+H)+.
後処理
- customThe reaction was quenched with 1 N HCl
- extractionextracted 3× with EtOAc
- washThe combined organic phases were washed with 1 N HCl
- dry with materialdried over sodium sulfate
- concentrationconcentrated in-vacuo
出典と根拠
- ORDレコード
- ord-ff8097910751497a8bf0bbbc0b01a8aa
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07985861B2
反応ノート
読み込み中…