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
To a suspension of lithium aluminum hydride (1.9 g) in anhydrous tetrahydrofuran (50 ml) is added dropwise with stirring a solution of 6-(3-azidopropoxy)carbostyril (10 g) in anhydrous tetrahydrofuran (200 ml) under ice-cooling. The mixture is stirred at room temperature for one hour, and thereto are added dropwise water (2 ml), a 15% aqueous sodium hydroxide solution (2 ml) and water (6 ml). The insoluble materials are collected by filtration, and added to a mixture of chloroform-methanol (8: 1). The mixture is heated, and then cooled. The insoluble material are removed by filtration. The filtrate is concentrated under reduced pressure to remove the solvent, and thereto is added diethyl ether. The precipitated crystals are collected by filtration to give 6-(3-aminopropoxy)carbostyril (6.2 g) as a white powder.
WORKUP
后处理
- additionis added dropwise
- temperaturecooling
- filtrationThe insoluble materials are collected by filtration
- additionadded to a mixture of chloroform-methanol (8: 1)
- temperatureThe mixture is heated
- temperaturecooled
- customThe insoluble material are removed by filtration
- concentrationThe filtrate is concentrated under reduced pressure
- customto remove the solvent
- additionis added diethyl ether
- filtrationThe precipitated crystals are collected by filtration