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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To the active ester thus obtained there is added a solution of 3.8 g of 3-[3-(3-methylpiperidinomethyl)phenoxy]propylamine in 70 ml of methanol and the mixture is stirred 3 hours at 50° C. The solvent is evaporated, the residue is taken up with 30 ml of N hydrochloric acid and the acid solution is washed 3 times with 20 ml of ethyl acetate. The pH is adjusted to 7.8, then the solution is salted out with sodium chloride and extracted 6 times with 30 ml of ethyl acetate. The organic extracts are collected and dried over anhydrous sodium sulfate and the solvent in evaporated to dryness. The product is purified by chromatography on silica as described in Example 7. Thus, the N-[3-[3-(3-methylpiperidinomethyl)phenoxy]propyl]-3-pyridinecarboxamide 1-oxide is obtained, identical to the product of Example 8.
WORKUP
后处理
- customThe solvent is evaporated
- washthe acid solution is washed 3 times with 20 ml of ethyl acetate
- extractionextracted 6 times with 30 ml of ethyl acetate
- customThe organic extracts are collected
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent in evaporated to dryness
- customThe product is purified by chromatography on silica