HRID579754

反应详情

EQUATION

反应方程式

HRID 579754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 200 mg of 5H-dibenzo[a,d]cyclohepten-5-ol, 300 mg of 4-[4-(4-fluorophenyl)-1-piperazinyl]butyramide and 8 ml of acetic acid is stirred at 70° C. for 20 hours. The acetic acid is distilled off under reduced pressure and 100 ml of chloroform is added to the residue. The solution is washed successively with 10% aqueous potassium carbonate solution, water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate, and the chrloroform is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (100:3) to give 250 mg of the title compound. m.p. 233°-235° C. (recrystallized from chloroform-n-hexane);

WORKUP

后处理

  1. distillationThe acetic acid is distilled off under reduced pressure and 100 ml of chloroform
  2. additionis added to the residue
  3. washThe solution is washed successively with 10% aqueous potassium carbonate solution, water and saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. distillationthe chrloroform is distilled off
  6. customThe residue is chromatographed on silica gel with chloroform-methanol (100:3)