HRID1251913

反应详情

EQUATION

反应方程式

HRID 1251913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2-chloropyridin-3-carboxylate (6.8 g.), 4-fluorobenzeneboronic acid (7.2 g.), 1M. aqueous sodium carbonate (40 ml.), Pd(dppb)Cl2(1.2 g.), ethanol(10 ml.) and toluene(150 ml.) was stirred at reflux under an inert atmosphere for 5 hr. The reaction was then cooled, the oganic layer separated, the aqueous extracted with toluene and then the Icombined extracts dried and evaporated to dryness. The product was purified by flash column chromatography eluting wth ethyl acetate/iso-hexane(9:1,8:2,7:3) to give methyl 2-(4-fluorophenyl)pyridin-3-carboxylate as a white solid(7.5 g.)

WORKUP

后处理

  1. temperatureat reflux under an inert atmosphere for 5 hr
  2. temperatureThe reaction was then cooled
  3. customthe oganic layer separated
  4. extractionthe aqueous extracted with toluene
  5. customthe Icombined extracts dried
  6. customevaporated to dryness
  7. customThe product was purified by flash column chromatography
  8. washeluting wth ethyl acetate/iso-hexane(9:1,8:2,7:3)