Urea → 7-Bromoquinazoline-2,4(1H,3H)-dione
反応式
[NH2:1][C:2]1[CH:10]=[C:9]([Br:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].[NH2:12][C:13](N)=[O:14]>O>[Br:11][C:9]1[CH:10]=[C:2]2[C:3]([C:4](=[O:5])[NH:12][C:13](=[O:14])[NH:1]2)=[CH:7][CH:8]=1参加物
4
反応条件
- 温度
- 195 °C
実験手順
To a 250 mL round bottom flask, 2-amino-4-bromo-benzoic acid (10 g, 0.0463 mol) and urea (27.78 g, 0.4629 mol) were added. The reaction mixture was stirred at 195° C. for 3 h. The reaction mixture was allowed to reach 80° C. and water was added. The aqueous reaction mixture was stirred at 80° C. for 5-10 min then allowed to reach room temperature. The solid was filtered, dried and azeotroped with toluene to afford the title compound [10 g, 90%]. This material was taken to the next step without any further purification.
後処理
- customto reach 80° C.
- stirringThe aqueous reaction mixture was stirred at 80° C. for 5-10 min
- customto reach room temperature
- filtrationThe solid was filtered
- customdried
- customazeotroped with toluene
出典と根拠
- ORDレコード
- ord-d5eaaefa4510494ebc20720a801c1112
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440662B2
反応ノート
読み込み中…