Phosphorus oxychloride → 4-Chloro-7-methoxy-quinazoline
反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](O)=[N:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:7]1[C:6]2[C:11](=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[N:10]=[CH:9][N:8]=1参加物
3
実験手順
Step 2 A suspension of 7-methoxyquinazolin-4-ol (400 mg, 2.271 mmol) in phosphorus oxychloride (7 mL, 75 mmol) was heated at reflux for 3 h. The solution was concentrated and the residue was suspended in EtOAc and stirred on an ice bath with NaHCO3 (aq) until all the solid was dissolved and gas evolution ceased. The layers were separated and the organic phase was dried and concentrated to provide 4-chloro-7-methoxyquinazoline as a light yellow-tan solid (438 mg, 99%). 1H NMR (400 MHz, chloroform-d) δ 8.94 (1 H, s), 8.15 (1 H, d, J=9.7 Hz), 7.29-7.37 (2 H, m), 4.00 (3 H, s).
後処理
- temperaturewas heated
- temperatureat reflux for 3 h
- concentrationThe solution was concentrated
- dissolutionwas dissolved
- customThe layers were separated
- customthe organic phase was dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6e27e0dba65e41c788ae4ac3843e316e
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08362065B2
反応ノート
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