Reaction #2487449

Reaction equation

2-Amino-4-trifluoromethylbenzoic acid

urea

→

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

Solvents

water

Conditions

Workup

1. 1
   Temperatureto cool to 100° C.
2. 2
   Temperatureto cool to room temperature
3. 3
   Otherthe solid was isolated by vacuum filtration
4. 4
   Washwashing with water (500 mL)
5. 5
   OtherThe solid was then dried under vacuum (10 mbar, 50° C.)
6. 6
   Other2.1 min, 230 (M+)

Procedure

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