HRID856058

反应详情

EQUATION

反应方程式

HRID 856058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-benzylpiperazin-1-yl-amine (43.18 g, 225 mmol) in etanol (400 ml), a suspension of 20% palladium hydroxide/carbon (6.50 g) in etanol (30 ml) was added, and the mixture was stirred at room temperature under an atmospheric pressure of hydrogen for 3 hours and then at 50° C. for 2 hours. The reaction mixture was filtered through Celite, 4-(trifluoromethoxy)benzaldehyde (42.92 g, 225 mmol) was added to the filtrate, and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1) to afford piperazin-1-yl-(4-trifluoromethoxybenzylidene)amine (56.88 g, yield 93%) as a pale yellow crystalline powder.

WORKUP

后处理

  1. additionwas added
  2. additionwas added to the filtrate
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1)