HRID2400264

反应详情

EQUATION

反应方程式

HRID 2400264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

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+).

WORKUP

后处理

  1. temperatureThe reaction mixture was then heated
  2. temperatureat reflux for 24 h
  3. customthe precipitate was isolated by vacuum filtration
  4. washwashing with water (3×500 mL)
  5. customdried under vacuum (10 mbar, 50° C.)
  6. custom3.7 min, 325 (M+)