HRID430487

反应详情

EQUATION

反应方程式

HRID 430487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

7 g (31.5 mmol) of methyl 4-fluoro-3-trifluoromethyl-benzoate are dissolved in 60 ml of dry dimethylsulphoxide (DMSO) and combined with 5.55 g (31.5 mmol) of N-benzylpiperazine and 4.35 g (31.5 mmol) of potassium carbonate. The mixture is stirred for 12 hours at 90° C. After cooling, the reaction mixture is poured into 200 ml of water and extracted three times with ethyl acetate. The combined organic phases are washed with water and saturated sodium chloride solution, dried over magnesium sulphate and distilled off in vacuo. The residue is chromatographed on silica gel with a mixture of ethyl acetate and n-heptane.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted three times with ethyl acetate
  3. washThe combined organic phases are washed with water and saturated sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. distillationdistilled off in vacuo
  6. customThe residue is chromatographed on silica gel with a mixture of ethyl acetate and n-heptane