Réaction #2487449

Équation de réaction

2-Amino-4-trifluoromethylbenzoic acid

urea

→

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

Solvants

water

Conditions de réaction

Traitement

1. 1
   Températureto cool to 100° C.
2. 2
   Températureto cool to room temperature
3. 3
   Autrethe solid was isolated by vacuum filtration
4. 4
   Lavagewashing with water (500 mL)
5. 5
   AutreThe solid was then dried under vacuum (10 mbar, 50° C.)
6. 6
   Autre2.1 min, 230 (M+)

Mode opératoire

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).

Source