HRID261949

反应详情

EQUATION

反应方程式

HRID 261949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

At a temperature of -10° C., 27.5 g. (0.25 mol) of ethyl chloroformate was added drop-wise to a solution of 28 g. (0.25 mol) of 1-(methoxymethyl)imidazole and 25 g. (0.25 mol) of triethylamine in 125 ml. of anhydrous chloroform. The mixture was stirred at 0° C. and then kept standing for two days at room temperature. The precipitated triethylamine hydrochloride was filtered off and washed with diethyl ether. The filtrate was concentrated by evaporating the solvents and the residue was dissolved in diethyl ether. The solution was dried over sodium sulphate, the ether was distilled off and the residue was distilled. The ethyl ester of 1-(methoxymethyl)imidazole-2-carboxylic acid was obtained. Boiling point 120°-124°/2 mm. Hg.

WORKUP

后处理

  1. customAt a temperature of -10° C., 27.5 g
  2. filtrationThe precipitated triethylamine hydrochloride was filtered off
  3. washwashed with diethyl ether
  4. concentrationThe filtrate was concentrated
  5. customby evaporating the solvents
  6. dissolutionthe residue was dissolved in diethyl ether
  7. dry with materialThe solution was dried over sodium sulphate
  8. distillationthe ether was distilled off
  9. distillationthe residue was distilled