反应 #2487449

反应方程式

2-Amino-4-trifluoromethylbenzoic acid

urea

→

7-Trifluoromethyl-1H-quinazoline-2,4-dione

溶剂

water

反应条件

后处理

1. 1
   温度to cool to 100° C.
2. 2
   温度to cool to room temperature
3. 3
   其他the solid was isolated by vacuum filtration
4. 4
   洗涤washing with water (500 mL)
5. 5
   其他The solid was then dried under vacuum (10 mbar, 50° C.)
6. 6
   其他2.1 min, 230 (M+)

实验过程

2-Amino-4-trifluoromethylbenzoic acid (25.0 g, 122 mmol) and urea (75.0 g, 1.2 mol) were combined and heated at 200° C. while stirring. After 1 h, the reaction mixture was allowed to cool to 100° C. and water (100 mL) was added. The reaction mixture was then allowed to cool to room temperature and the solid was isolated by vacuum filtration washing with water (500 mL). The solid was then dried under vacuum (10 mbar, 50° C.). Yield=24 g, 86%; LC-MS: 2.1 min, 230 (M+); 1H NMR (DMSO-d6) δ 7.44 (s, 1 H) 7.47 (d, 1 H), 8.07 (d, 1 H), 11.43 (br s, 1 H), 11.56 (br s, 1 H).

来源