반응식
[CH2:1]([C:3]1[C:4](=[O:14])[NH:5][C:6]2[C:11]([N:12]=1)=[CH:10][CH:9]=[C:8]([F:13])[CH:7]=2)[CH3:2].[Br:15]N1C(C)(C)C(=O)N(Br)C1=O.C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>>[Br:15][CH:1]([C:3]1[C:4](=[O:14])[NH:5][C:6]2[C:11]([N:12]=1)=[CH:10][CH:9]=[C:8]([F:13])[CH:7]=2)[CH3:2]참가 물질
6
반응 조건
- 온도
- 80 °C
실험 절차
3-Ethyl-7-fluoroquinoxalin-2(1H)-one (20.61 g, 107.2 mmol) and 1,3-dibromo-5,5-dimethylhydantoin (18.77 g, 64.34 mmol) suspended in carbon tetrachloride (1072 ml, 107.2 mmol). To the heterogeneous mixture was added benzoyl peroxide (3.463 g, 10.72 mmol) and the mixture was heated at reflux with stirring (oil bath temperature: 80° C.) for 20 h. After 20 h, the mixture was cooled to rt. After cooling, the mixture was poured into saturated aqueous sodium bicarbonate solution (1 L) with stirring. The precipitate was collected by filtration and washed with water (1 L) to give 3-(1-bromoethyl)-7-fluoroquinoxalin-2(1H)-one (23.19 g, 79.8% yield) as a tan solid:
후처리
- temperaturethe mixture was heated
- temperatureat reflux
- waitAfter 20 h
- temperaturethe mixture was cooled to rt
- temperatureAfter cooling
- stirringwith stirring
- filtrationThe precipitate was collected by filtration
- washwashed with water (1 L)
출처 및 근거
- ORD 기록
- ord-ae08bcbc30f44f089ad7b8d076fba8d7
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08716290B2
연결된 노트
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