反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated for six hours
- filtrationThe reaction mixture is filtered on diatomaceous earth
- washthe filter residue is washed with diethyl ether
- additionthe filtrate is mixed with 1.5 ml of 2n hydrochloric acid
- stirringstirred for 4 hours at room temperature
- customThe organic phase is separated
- dry with materialdried with sodium sulfate
- concentrationconcentrated by evaporation