Bromine → 5-Bromo-8-methoxy-2-methylquinoline
반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]=[C:10]([CH3:13])[CH:9]=[CH:8]2.[Br:14]Br>CO>[Br:14][C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[C:12]2[C:7]=1[CH:8]=[CH:9][C:10]([CH3:13])=[N:11]2참가 물질
4
반응 조건
- 온도
- 45 °C
실험 절차
A solution of 8-methoxy-2-methylquinoline (1.0 g) in methanol (30 ml) was treated at room temperature with bromine (0.31 ml). The mixture was heated at 45° C. for 2 hours and the reaction quenched with 5% aqueous sodium metabisulphite (50 ml). The solution was basified with 25% aqueous sodium hydroxide to pH13 and the product extracted with ethyl acetate (2×100 ml). The extracts were combined, dried over magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was dissolved in ethyl acetate and passed through a silica pad. The solution was evaporated in vacuo to yield the desired product as an off-white solid (0.43 g).
후처리
- customthe reaction quenched with 5% aqueous sodium metabisulphite (50 ml)
- extractionthe product extracted with ethyl acetate (2×100 ml)
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customthe filtrate evaporated in vacuo
- dissolutionThe residue was dissolved in ethyl acetate
- customThe solution was evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-f7019cba75f449349a0c7c8c68bde685
- 출처 데이터셋
- uspto-grants-1998_09
- 특허 번호
- US05804588
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