HRID2288516

反应详情

EQUATION

反应方程式

HRID 2288516 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-methyl-imidazole and 5-hydroxymethyl-2-methoxymethyl-1-methyl-imidazole and 7.3 g (55 mmol) of N-chloro-succinimide was heated to 50° C. in 48 ml of ethylene glycol monoethylether and 70 ml of dioxan 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)