HRID1420576

反应详情

EQUATION

反应方程式

HRID 1420576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of N-(2-trifluoromethylphenyl)cyclohexanecarboxamide (0.2 g) (compd 26A), 1-(2-chloroethyl)-4-(2-methoxyphenyl)piperazine (0.37 g), 50% (w/w) NaOH (0.5 mL), TEBAC (0.16 g) and toluene (2 mL) was stirred at 80° C. for 3.5 h. An additional amount of compd 26A (0.2 g) was then added and after 6 h stirring at 80° C. The mixture was poured into H2O and extracted with CH2Cl2. The organic phase was dried on anhydrous Na2SO4, evaporated to dryness and the residue purified by flash chromatography (EtOAc-petroleum ether 3:7) giving 0.12 g (17%) of the title compound.

WORKUP

后处理

  1. stirringstirring at 80° C
  2. extractionextracted with CH2Cl2
  3. dry with materialThe organic phase was dried on anhydrous Na2SO4
  4. customevaporated to dryness
  5. customthe residue purified by flash chromatography (EtOAc-petroleum ether 3:7)