HRID55264

反应详情

EQUATION

反应方程式

HRID 55264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of 495 mg of 3-{6-iodo-3-[6-(4-methoxyphenyl-(5E)-5-hexenyloxy]-2-pyridyl}-propionic acid methyl ester and 397 mg of ethoxyvinyltributyltin in 2 ml of toluene is mixed with 30 mg of bis-triphenylphosphine-palladium(II) chloride and heated for six hours with stirring to 110° C. The reaction mixture is filtered on diatomaceous earth, the filter residue is washed with diethyl ether, the filtrate is mixed with 1.5 ml of 2n hydrochloric acid and stirred for 4 hours at room temperature. The organic phase is separated, dried with sodium sulfate and concentrated by evaporation. 95 mg of 3-{6-acetyl-3-[6-(4-methoxyphenyl-(5E)-5-hexenyloxy]-2-pyridyl}-propionic acid methyl ester is obtained as oil.

WORKUP

后处理

  1. temperatureheated for six hours
  2. filtrationThe reaction mixture is filtered on diatomaceous earth
  3. washthe filter residue is washed with diethyl ether
  4. additionthe filtrate is mixed with 1.5 ml of 2n hydrochloric acid
  5. stirringstirred for 4 hours at room temperature
  6. customThe organic phase is separated
  7. dry with materialdried with sodium sulfate
  8. concentrationconcentrated by evaporation