HRID443817
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
- 20 °C
PROCEDURE
实验过程
A mixture of 3-chloromethylisoquinoline hydrochloride (96 g) and sodium methoxide (80 g) in methanol (1.5 liters) is heated under reflux for 8 hours. After cooling to 20° C., the mixture is filtered and the filtrate is evaporated to dryness at 50° C. under reduced pressure (20 mm Hg). The residue is taken up in methylene chloride (1 liter), the mixture is washed with water (3×150 cc), the organic phase is dried over magnesium sulphate and filtered, and the filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg). The oily residue is distilled at 82° C. under reduced pressure (0.6 mm Hg). 3-Methoxymethylisoquinoline (68 g), a colourless oil, is obtained.
WORKUP
后处理
- temperatureis heated
- temperatureunder reflux for 8 hours
- filtrationthe mixture is filtered
- customthe filtrate is evaporated to dryness at 50° C. under reduced pressure (20 mm Hg)
- washthe mixture is washed with water (3×150 cc)
- dry with materialthe organic phase is dried over magnesium sulphate
- filtrationfiltered
- customthe filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg)
- distillationThe oily residue is distilled at 82° C. under reduced pressure (0.6 mm Hg)