HRID1095303

反应详情

EQUATION

反应方程式

HRID 1095303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1.0 mmol of ethyl (1-trityl-1H-imidazol-4-ylmethoxy)acetate in 16 ml of tetrahydrofuran and 16 ml of 2N NaOH is stirred under reflux for 18 hours. The reaction mixture is cooled and the tetrahydrofuran is distilled off. 20 ml of 2N HCl are added to the aqueous residue, and the resulting suspension is diluted with tert-butyl methyl ether. The solid is filtered off and the filter cake is washed with water and tert-butyl methyl ether and dried. The title compound is obtained as a yellowish solid. Rf=0.02 (ethyl acetate-heptane 2:1); Rt=3.86 (gradient I).

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. temperatureThe reaction mixture is cooled
  3. distillationthe tetrahydrofuran is distilled off
  4. addition20 ml of 2N HCl are added to the aqueous residue
  5. additionthe resulting suspension is diluted with tert-butyl methyl ether
  6. filtrationThe solid is filtered off
  7. washthe filter cake is washed with water and tert-butyl methyl ether
  8. customdried