HRID1856755

反应详情

EQUATION

反应方程式

HRID 1856755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-(3-Chloropropoxy)carbostyril (20 g) is added into a 40% solution of methylamine in methanol (200 ml), and the mixture is heated with stirring at 100° C. overnight in a sealed tube. The mixture is concentrated under reduced pressure to remove the solvent, and the precipitated crystals are washed with a mixture of chloroform-diethyl ether, purified by silica gel column chromatography (solvent; methylene chloride:methanol:aqueous ammonia=50:10:1), and recrystallized from chloroform-diethyl ether to give 6-(3-methylaminopropoxy)carbostyril (15.4 g).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. concentrationThe mixture is concentrated under reduced pressure
  3. customto remove the solvent
  4. washthe precipitated crystals are washed with a mixture of chloroform-diethyl ether
  5. custompurified by silica gel column chromatography (solvent; methylene chloride:methanol:aqueous ammonia=50:10:1)
  6. customrecrystallized from chloroform-diethyl ether