HRID1199986

反应详情

EQUATION

反应方程式

HRID 1199986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 4-fluorobenzoylacetate (0.78 g, 4 mM) and 4-(2-methylimidazo[4,5-c]pyrid-1-yl)butanol (0.82 g, 4 mM--see Preparation 16) were heated at reflux in toluene (100 cm3) allowing the toluene to reduce to about 20 cm3 over a period of 2 hours. The remaining toluene was removed in vacuo and the residue purified by column chromatography on silica (Merck "Kieselgel 60"--Trade Mark) eluting with dichloromethane:methanol 19:1. Evaporation of the appropriate fractions gave the title compound as a colourless oil, (1.05 g, 71%).

WORKUP

后处理

  1. customThe remaining toluene was removed in vacuo
  2. customthe residue purified by column chromatography on silica (Merck "Kieselgel 60"--Trade Mark)
  3. washeluting with dichloromethane:methanol 19:1
  4. customEvaporation of the appropriate fractions