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