반응식
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N:17]=[CH:18]2.CO>ClCCl>[ClH:1].[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N+:17]([O-:9])=[CH:18]2참가 물질
5
실험 절차
m-Chloroperbenzoic acid (1.4 g, 75%) was added in portions to a stirred solution of 5-bromo-6-methoxyisoquinoline (12 g, 5.04 mmol) in dichloromethane (12 ml). The mixture was stirred for 1 h then further dichloromethane (10 ml) added and the mixture stirred for an additional 2 h. Methanol (12 ml) was added and the mixture concentrated in vacuo to ˜9 ml, then 1M hydrochloric acid in diethyl ether (10 ml) was added. The mixture was diluted with ether and filtered, the precipitated solid was washed with diethyl ether and dried in vacuo to give crude 5-bromo-6-methoxyisoquinoline-N-oxide hydrochloride (1.22 g).
후처리
- stirringthe mixture stirred for an additional 2 h
- concentrationthe mixture concentrated in vacuo to ˜9 ml
- addition1M hydrochloric acid in diethyl ether (10 ml) was added
- additionThe mixture was diluted with ether
- filtrationfiltered
- washthe precipitated solid was washed with diethyl ether
- customdried in vacuo
출처 및 근거
- ORD 기록
- ord-a3cddaab01a94e84accae8268c62de9f
- 출처 데이터셋
- uspto-grants-2009_11
- 특허 번호
- US07618985B2
연결된 노트
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