HRID596851

反应详情

EQUATION

反应方程式

HRID 596851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

31 g. of 1-(4'-chloro benzyl)-2-phenyl piperazine prepared according to Example B), 25 g. of piperidino ethylchloride, 20 g. of triethylamine, and 250 cc. of acetone are boiled under reflux for 18 hours. The filtered reaction solution is freed of its solvent by concentration by evaporation. The residue is dissolved in benzene. The benzene solution is washed with water. After drying and distilling off the solvent, the base is obtained in the form of a viscous, yellow oil on distillation at 210° C./0.06 Torr. The oil crystallizes on trituration with isopropanol. After twice recystallizing the crystals from n-heptane (41 g. of yellow crystals of the melting point 85°-87° C.) are obtained. The yield is 95 % of the theoretical yield.

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. customThe filtered reaction solution
  3. concentrationis freed of its solvent by concentration by evaporation
  4. dissolutionThe residue is dissolved in benzene
  5. washThe benzene solution is washed with water
  6. customAfter drying
  7. distillationdistilling off the solvent
  8. customthe base is obtained in the form of a viscous, yellow oil
  9. distillationon distillation at 210° C./0.06 Torr
  10. customThe oil crystallizes on trituration with isopropanol
  11. customof yellow crystals of the melting point 85°-87° C.) are obtained