HRID232034

反应详情

EQUATION

反应方程式

HRID 232034 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

2-Methylimidazo[4,5-c]pyridine (10.6 g) was mixed with ethylene carbonate (8.3 g) and heated as a melt at 150° C. for 1/2 hour. The crude black product was chromatographed on silica eluting with 40% methanol in ethyl acetate. The fraction with Rf 0.33 in methanol, ethyl acetate, (2:3) was evaporated and was identified as a mixture of the title compound and of the isomeric 1-(2-hydroxyethyl)-2-methylimidazo[4,5-c]pyridine. The mixture was chromatographed on silica eluting with 20% methanol in acetone. Fractions containing the more mobile isomer were combined and evaporated yielding the title compound (1.22 g, 9%) as a foam.

WORKUP

后处理

  1. customThe crude black product was chromatographed on silica eluting with 40% methanol in ethyl acetate
  2. customThe fraction with Rf 0.33 in methanol, ethyl acetate, (2:3) was evaporated
  3. additionwas identified as a mixture of the title compound and of the isomeric 1-(2-hydroxyethyl)-2-methylimidazo[4,5-c]pyridine
  4. customThe mixture was chromatographed on silica eluting with 20% methanol in acetone
  5. additionFractions containing the more mobile isomer
  6. customevaporated