HRID1856755
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
- 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
- temperaturethe mixture is heated
- concentrationThe mixture is concentrated under reduced pressure
- customto remove the solvent
- washthe precipitated crystals are washed with a mixture of chloroform-diethyl ether
- custompurified by silica gel column chromatography (solvent; methylene chloride:methanol:aqueous ammonia=50:10:1)
- customrecrystallized from chloroform-diethyl ether