HRID1856750

反应详情

EQUATION

反应方程式

HRID 1856750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionis added dropwise
  2. temperaturecooling
  3. filtrationThe insoluble materials are collected by filtration
  4. additionadded to a mixture of chloroform-methanol (8: 1)
  5. temperatureThe mixture is heated
  6. temperaturecooled
  7. customThe insoluble material are removed by filtration
  8. concentrationThe filtrate is concentrated under reduced pressure
  9. customto remove the solvent
  10. additionis added diethyl ether
  11. filtrationThe precipitated crystals are collected by filtration