Phosphorus oxychloride → 6-Bromo-2-chloro-5-fluoroquinazoline
反応式
[Br:1][C:2]1[C:3]([F:13])=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7](O)[N:6]=[CH:5]2.P(Cl)(Cl)([Cl:16])=O>>[Br:1][C:2]1[C:3]([F:13])=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([Cl:16])[N:6]=[CH:5]2参加物
3
実験手順
A solution of 6-bromo-5-fluoroquinazolin-2-ol (3.0 g, 12.34 mmol) in phosphoryl trichloride (10 mL) was refluxed at 135° C. for 5 hours. Most of phosphoryl trichloride was removed under reduced pressure, and the residue was dropwise added to ice water (200 mL). The resulting precipitate was collected via filtration as a yellow solid (3.1 g, 96%). MS (ES+) C8H3BrClFN2 requires: 260, found: 261, 263 [M+H]+.
後処理
- customMost of phosphoryl trichloride was removed under reduced pressure
- additionthe residue was dropwise added to ice water (200 mL)
- filtrationThe resulting precipitate was collected via filtration as a yellow solid (3.1 g, 96%)
出典と根拠
- ORDレコード
- ord-553c038ce2194e5d9578df75645dda80
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434700B2
反応ノート
読み込み中…