반응 #2487449

반응 방정식

2-Amino-4-trifluoromethylbenzoic acid

urea

→

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

용매

water

반응 조건

후처리

1. 1
   온도to cool to 100° C.
2. 2
   온도to cool to room temperature
3. 3
   기타the solid was isolated by vacuum filtration
4. 4
   세척washing with water (500 mL)
5. 5
   기타The solid was then dried under vacuum (10 mbar, 50° C.)
6. 6
   기타2.1 min, 230 (M+)

실험 절차

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).

출처