Dimethylamine → 3-(N,N-dimethylsulfamoyl)benzoic acid
반응식
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]참가 물질
5
실험 절차
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)+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-629b952ef93e4ff481ffe8af23b694ca
- 출처 데이터셋
- uspto-grants-2009_10
- 특허 번호
- US07601844B2
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