Reacción #2487446

ord-3b8ceb7c0ee94b25a4d0257f0dc80bd9

Ecuación de reacción

NC(=O)c1ccc(C(F)(F)F)cc1N
2-amino-4-(trifluoromethyl)benzamide
O=Cc1ccc(Cl)cc1
4-chlorobenzaldehyde
O=c1[nH]c(-c2ccc(Cl)cc2)nc2cc(C(F)(F)F)ccc12
2-(4-Chlorophenyl)-7-trifluoromethyl-3H-quinazolin-4-one

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture was then heated
  2. 2
    Temperaturaat reflux for 24 h
  3. 3
    Otrothe precipitate was isolated by vacuum filtration
  4. 4
    Lavadowashing with water (3×500 mL)
  5. 5
    Otrodried under vacuum (10 mbar, 50° C.)
  6. 6
    Otro3.7 min, 325 (M+)

Procedimiento

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+).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08796180B2uspto-grants-2014_08