反应 #2487446

ord-3b8ceb7c0ee94b25a4d0257f0dc80bd9

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was then heated
  2. 2
    温度at reflux for 24 h
  3. 3
    其他the precipitate was isolated by vacuum filtration
  4. 4
    洗涤washing with water (3×500 mL)
  5. 5
    其他dried under vacuum (10 mbar, 50° C.)
  6. 6
    其他3.7 min, 325 (M+)

实验过程

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+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08796180B2uspto-grants-2014_08