HRID723406

反应详情

EQUATION

反应方程式

HRID 723406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.2 g of 8-benzyloxy-6-hydroxymethyl-2,3-dimethylimidazo[1,2-a]pyridine in 12 ml of dimethylformamide is treated with 0.36 g of 60% strength sodium hydride in paraffin under an inert gas atmosphere, stirred for 30 minutes at room temperature until the evolution of gas is complete, and then treated at room temperature with 0.56 ml of methyl iodide. After a reaction time of one hour, it is poured onto 100 ml of ice water and extracted 3 times with 100 ml of ethyl acetate each time. The organic phases are combined and washed with water. The solvent is stripped off in vacuo and the oily residue is chromatographed on silica gel (eluent: methylene chloride/methanol=100/1). 0.34 g of the title compound of melting point 107° C. (diethyl ether) is obtained.

WORKUP

后处理

  1. extractionextracted 3 times with 100 ml of ethyl acetate each time
  2. washwashed with water
  3. customthe oily residue is chromatographed on silica gel (eluent: methylene chloride/methanol=100/1)