Phosphorus oxychloride → 6-Bromo-2-chloroquinazoline
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7](O)[N:6]=[CH:5]2.P(Cl)(Cl)([Cl:15])=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([Cl:15])[N:6]=[CH:5]2参加物
3
実験手順
A solution of 6-bromoquinazolin-2-ol (9.72 g, 40 mmol) in phosphorus oxychloride (100 mL) was refluxed for 5 h. LCMS showed the reaction was completed. The reaction was cooled to RT, and most of phosphorus oxychloride was removed under reduced pressure. The residue was dropwise added to ice water (500 mL), and the resulting precipitate was collected by the filtration to give the title compound (9 g, 87%) as a yellow solid. MS (ES+) C8H3BrClFN2 requires: 260, 262. found: 261, 263 [M+H]+.
後処理
- custommost of phosphorus oxychloride was removed under reduced pressure
- additionThe residue was dropwise added to ice water (500 mL)
- filtrationthe resulting precipitate was collected by the filtration
出典と根拠
- ORDレコード
- ord-d3e4c7cb6b9b4efa9c373e221090e763
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09340514B2
反応ノート
読み込み中…