Water → 7-bromo-2H,3H,4H-pyrido(3,2-b)(1,4)oxazin-3-one
反応式
[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]=1参加物
5
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-4f8809ff4734481483f2d98139dedaaa
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09090561B2
反応ノート
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