HRID2295442

反应详情

EQUATION

反应方程式

HRID 2295442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8.78 g of trans-4-(4-chlorophenoxy)-1-ethoxycarbonyl-3-phenylpiperidine, 64 ml of 20% aqueous NaOH solution and 125 ml of absolute ethanol is refluxed for 18 hours under nitrogen. The ethanol is then removed in vacuo and the aqueous residue is partitioned between dichloromethane and distilled water. The aqueous phase is extracted with dichloromethane, and the combined organic extracts are then washed with water, saturated aqueous NaCl solution, dried over anhydrous Na2SO4 and concentrated in vacuo to afford a solid which is recrystallized from cyclohexane to yield trans-4-(4-chlorophenoxy)-3-phenylpiperidine, mp 101.5°-103° C.

WORKUP

后处理

  1. temperatureis refluxed for 18 hours under nitrogen
  2. customThe ethanol is then removed in vacuo
  3. customthe aqueous residue is partitioned between dichloromethane
  4. distillationdistilled water
  5. extractionThe aqueous phase is extracted with dichloromethane
  6. washthe combined organic extracts are then washed with water, saturated aqueous NaCl solution
  7. dry with materialdried over anhydrous Na2SO4
  8. concentrationconcentrated in vacuo
  9. customto afford a solid which
  10. customis recrystallized from cyclohexane