HRID657607
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe suspension is filtrated
- washthe precipitate washed with ethanol
- concentrationThe filtrate is concentrated under reduced pressure
- custompurified by chromatography over silica gel with a gradient of dichloromethane/methanol from 98/2 to 90/10
- additionFraction containing the expected products
- concentrationconcentrated under reduced pressure