HRID50379

反应详情

EQUATION

反应方程式

HRID 50379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1:1 mixture of 7.7 g (49 mmol) of 4-hydroxymethyl-2-methoxymethyl-1-methylimidazole and 5-hydroxymethyl-2-methoxymethyl-1-methylimidazole and 7.3 g (55 mmol) of N-chlorosuccinimide was heated to 50° C. in 48 mL of ethylene glycol monoethylether and 70 mL of dioxane for 10 hours. Then the solvent was distilled off in vacuo and the crude product purified by chromatography (silica gel; methylene chloride/ethanol=99:1 to 90:10) to obtain the isomerically pure title compound. Yield: 3.4 g (36% of theory); Rf value: 0.40 (silica gel; methylene chloride/ethanol=19:1).

WORKUP

后处理

  1. distillationThen the solvent was distilled off in vacuo
  2. customthe crude product purified by chromatography (silica gel; methylene chloride/ethanol=99:1 to 90:10)