Chlorosulfonyl isocyanate → 6-Nitro-1H-indole-3-carbonitrile
반응식
[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[CH:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].ClS([N:17]=[C:18]=O)(=O)=O.C([O-])(O)=O.[Na+]>CN(C=O)C.CC#N>[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8]([C:18]#[N:17])=[CH:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]참가 물질
6
실험 절차
To a solution of 6-nitroindole (4.86 g 30 mmol) in DMF (24.3 mL) and CH3CN (243 mL) was added dropwise a solution of ClSO2NCO (5 mL, 57 mmol) in CH3CN (39 mL) at 0° C. After addition, the reaction was allowed to warm to room temperature and stirred for 2 h. The mixture was poured into ice-water, basified with sat. NaHCO3 solution to pH 7-8 and extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4 and concentrated to give 6-nitro-1H-indole-3-carbonitrile (4.6 g, 82%).
후처리
- additionAfter addition
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-1416c01d4a9f4ed5a1a1d158b4480070
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08829204B2
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