HRID644541

反应详情

EQUATION

反应方程式

HRID 644541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of aluminium trichloride (1.46 mmol, 195 mg) in dichloromethane (3 ml) was added dropwise N-methylpiperazine (1.83 mmol, 203 l). The resultant mixture was stirred for 0.5 h and to this, a solution of 3-(3-phenyl-6-trifluoromethyl-3H-benzimidazol-4-yl)acrylic acid methyl ester (0.73 mmol, 250 mg) was added dropwise. The resultant mixture stirred for 16 h at 60° C. Upon cooling, aqueous sodium carbonate (5%, 5 ml) was added and the mixture was shaken. The organic layer was isolated by filtration through a hydrophobic frit and evaporated under reduced pressure to give an off-white solid. Recrystallisation from diethyl ether afforded the title compound as a white powder (160 mg, 53%), m/z 415.2 (M+H)+.

WORKUP

后处理

  1. temperatureUpon cooling
  2. customThe organic layer was isolated by filtration through a hydrophobic frit
  3. customevaporated under reduced pressure
  4. customto give an off-white solid
  5. customRecrystallisation from diethyl ether