반응 #2487446

반응 방정식

2-amino-4-(trifluoromethyl)benzamide

4-chlorobenzaldehyde

→

2-(4-Chlorophenyl)-7-trifluoromethyl-3H-quinazolin-4-one

용매

water

반응 조건

후처리

1. 1
   온도The reaction mixture was then heated
2. 2
   온도at reflux for 24 h
3. 3
   기타the precipitate was isolated by vacuum filtration
4. 4
   세척washing with water (3×500 mL)
5. 5
   기타dried under vacuum (10 mbar, 50° C.)
6. 6
   기타3.7 min, 325 (M+)

실험 절차

To a stirred suspension of 2-amino-4-(trifluoromethyl)benzamide (33.6 g, 0.16 mol) in water (750 mL) was added dropwise 4-chlorobenzaldehyde. Iron trichloride hexahydrate (133 g) was then added in portions. The reaction mixture was then heated at reflux for 24 h. After allowing the suspension to cool to room temperature, the precipitate was isolated by vacuum filtration washing with water (3×500 mL) and dried under vacuum (10 mbar, 50° C.). Yield=50 g, 94%; HPLC-mass spectrometry (LC-MS): 3.7 min, 325 (M+).

출처