Réaction #2487446

ord-3b8ceb7c0ee94b25a4d0257f0dc80bd9

Équation de réaction

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

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe reaction mixture was then heated
  2. 2
    Températureat reflux for 24 h
  3. 3
    Autrethe precipitate was isolated by vacuum filtration
  4. 4
    Lavagewashing with water (3×500 mL)
  5. 5
    Autredried under vacuum (10 mbar, 50° C.)
  6. 6
    Autre3.7 min, 325 (M+)

Mode opératoire

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+).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08796180B2uspto-grants-2014_08