HRID1267966
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
3-(3-Methoxymethoxypyridin-4-yl)-1-propanol (3.67 g, 18.6 mmol) obtained in Example 2 is dissolved in ethanol (100 ml), and thereto is added a 15% aqueous hydrochloric acid solution (20 ml), and the mixture is heated under reflux for 30 minutes. The reaction solution is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate), and further recrystallized from diethyl ether to give the title compound (2.08 g) as colorless crystals, m.p. 123-126° C.
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureunder reflux for 30 minutes
- concentrationThe reaction solution is concentrated under reduced pressure
- customthe residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate)
- customfurther recrystallized from diethyl ether