HRID1086242

反应详情

EQUATION

反应方程式

HRID 1086242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 300 mg of 1-[bis(4-fluorophenyl)methyl]-3-methylpiperazine and 252 mg of N-(2,4,6-trimethylphenyl) chloroacetamide was dissolved in 20 ml of a 1:1 by volume mixture of tetrahydrofuran and N,N-dimethylformamide. 100 mg of anhydrous potassium carbonate were then added to the solution, and the reaction mixture was stirred at 70° C. for 3 hours, after which ethyl acetate was added to it and the organic layer was separated. The organic layer was washed three times with water, and then dried over anhydrous magnesium sulfate. The solvent was then removed by evaporation under reduced pressure, and the residue was subjected to silica gel thin layer chromatography using a 1:1 by volume mixture of cyclohexane and ethyl acetate as the developing solvent, to afford a purified 1-[bis(4-fluorophenyl)methyl]-4-[(2,4,6-trimethylphenyl)carbamoylmethyl]-3-methylpiperazine.

WORKUP

后处理

  1. customthe organic layer was separated
  2. washThe organic layer was washed three times with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was then removed by evaporation under reduced pressure
  5. additionby volume mixture of cyclohexane and ethyl acetate as the developing solvent