Water → 6-Bromo-2-chloro-8-methoxyquinazoline
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:12][CH3:13])[CH:11]=1)[NH:8][C:7](=O)[N:6]=[CH:5]2.O.O=P(Cl)(Cl)[Cl:18]>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:12][CH3:13])[CH:11]=1)[N:8]=[C:7]([Cl:18])[N:6]=[CH:5]2参加物
4
実験手順
6-bromo-8-methoxy-1H-quinazolin-2-one (2.62 g, 10.27 mmol) is suspended in 30 mL POCl3 and refluxed for 30 min. The reaction mixture is stirred into water, while the temperature never exceeds 15° C. The aqueous phase is extracted with DCM, the organic phase is dried and 6-bromo-2-chloro-8-methoxy-quinazoline (HPLC-MS: tRet.=1.88 min, MS(M+H)+=273/275/277; method FSUN) is obtained.
後処理
- temperaturerefluxed for 30 min
- extractionThe aqueous phase is extracted with DCM
- customthe organic phase is dried
出典と根拠
- ORDレコード
- ord-3a2ade1bf8664602b86a7741802fd93e
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637549B2
反応ノート
読み込み中…