HRID657607

反应详情

EQUATION

反应方程式

HRID 657607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 4-(3-chloropropoxy)benzoate (4.57 g), potassium carbonate (8.29 g), cis and trans-3,5-dimethylpiperidine (5.31 mL) and a catalytic amount of potassium iodide in N,N-dimethylformamide (100 mL) is stirred overnight at 100° C. The suspension is filtrated and the precipitate washed with ethanol. The filtrate is concentrated under reduced pressure and purified by chromatography over silica gel with a gradient of dichloromethane/methanol from 98/2 to 90/10. Fraction containing the expected products are pooled and concentrated under reduced pressure yielding 5.33 g of cis and trans-1-{3-[4-(methoxycarbonyl)phenoxy]propyl}-3,5-dimethylpiperidine.

WORKUP

后处理

  1. filtrationThe suspension is filtrated
  2. washthe precipitate washed with ethanol
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. custompurified by chromatography over silica gel with a gradient of dichloromethane/methanol from 98/2 to 90/10
  5. additionFraction containing the expected products
  6. concentrationconcentrated under reduced pressure