Water → 7-bromo-2H,3H,4H-pyrido(3,2-b)(1,4)oxazin-3-one
반응식
[O:1]1[CH2:6][C:5](=[O:7])[NH:4][C:3]2[N:8]=[CH:9][CH:10]=[CH:11][C:2]1=2.C1C(=O)N([Br:19])C(=O)C1.O>CN(C=O)C>[Br:19][C:10]1[CH:9]=[N:8][C:3]2[NH:4][C:5](=[O:7])[CH2:6][O:1][C:2]=2[CH:11]=1참가 물질
5
실험 절차
To a solution of 2H-pyrido[3,2-b][1,4]oxazin-3-one (0.75 g, 5 mmol) in DMF (18 mL) was slowly added NBS (1.07 g, 6 mmol) under N2. The mixture was stirred at rt for 16 h. HPLC indicated 75% conversion. More NBS (0.53 g, 3 mmol) was added and the mixture was stirred for another 24 h. Water (5 mL) was added and the reaction flask was chilled. The white solid which separated was filtered and washed with EtOAc, H2O, Et2O, and dried under vacuum in the presence of P2O5 and then used directly in the next step (687 mg, 60%).
후처리
- stirringthe mixture was stirred for another 24 h
- temperaturethe reaction flask was chilled
- customThe white solid which separated
- filtrationwas filtered
- washwashed with EtOAc, H2O, Et2O
- dry with materialdried under vacuum in the presence of P2O5
출처 및 근거
- ORD 기록
- ord-4f8809ff4734481483f2d98139dedaaa
- 출처 데이터셋
- uspto-grants-2015_07
- 특허 번호
- US09090561B2
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