HRID258274
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
A suspension of 6-(2,3-epoxypropoxy)carbostyril (15 g) and N-methylbenzylamine (11 g) in methanol (150 ml) is heated with refluxing for 2.5 hours. From the mixture, methanol is distilled off under reduced pressure, and to the resulting residue is added diethylether and the precipitated crystals are collected by filtration. The crystals thus obtained are purified by silica gel column chromatography (solvent; methanol:chloroform=1:100-1:25), and recrystallized from ethanol to give 6-[3-(N-methyl-N-benzylamino)-2-hydroxypropoxy]carbostyril (7.6 g), as white powder, m.p. 129°-132° C.
WORKUP
后处理
- temperatureis heated
- temperaturewith refluxing for 2.5 hours
- distillationFrom the mixture, methanol is distilled off under reduced pressure
- additionto the resulting residue is added diethylether
- filtrationthe precipitated crystals are collected by filtration
- customThe crystals thus obtained
- customare purified by silica gel column chromatography (solvent; methanol:chloroform=1:100-1:25)
- customrecrystallized from ethanol