HRID53059

反应详情

EQUATION

反应方程式

HRID 53059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.20 g of methyl iodide were added dropwise to a mixture of 714 mg of magnesium in 30 ml of diethyl ether, under a nitrogen atmosphere, and the resulting solution was heated under reflux, whilst stirring, for 30 minutes. At the end of this time, a solution of 2.00 g of diethyl 2-ethylthioimidazole-4,5-dicarboxylate [prepared as described in step (i) above] in 20 ml of methylene chloride was added dropwise to the reaction solution, and the mixture was treated in a similar manner to that described in Preparation 49(ii). The resulting crystalline residue was washed with a mixture of hexane and diisopropyl ether, to give 1.32 g of the title compound, melting at 82°-85° C.

WORKUP

后处理

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux
  3. additionthe mixture was treated in a similar manner to that
  4. washThe resulting crystalline residue was washed with a mixture of hexane and diisopropyl ether