تفاعل #2487446

ord-3b8ceb7c0ee94b25a4d0257f0dc80bd9

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was then heated
  2. 2
    درجة الحرارةat reflux for 24 h
  3. 3
    أخرىthe precipitate was isolated by vacuum filtration
  4. 4
    غسيلwashing with water (3×500 mL)
  5. 5
    أخرىdried under vacuum (10 mbar, 50° C.)
  6. 6
    أخرى3.7 min, 325 (M+)

الإجراء التجريبي

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+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08796180B2uspto-grants-2014_08