反应详情

温度

100 °C

A solution of 41.8 ml (0.3 mol) of triethylamine and 8.6 ml (0.23 mol) of formic acid in 500 ml of dioxane is added to a solution of 43.5 g (0.09 mol) of diallyl 2-[2-(4-cyanophenyl)ethyl]-2-(4-methoxycarbonylbenzyl)malonate from Example 13A, 1.67 g (0.01 mol) of triphenylphosphine and 410 mg of palladium acetate in 505 ml of dioxane at room temperature. The reaction mixture is then stirred at 100° C. for 2 hours. After conversion is complete, the reaction solution is cooled and the solvent is removed in vacuo. The resulting residue is purified by flash chromatography on silica gel (mobile phase: dichloromethane/methanol 50:1). 25 g (0.074 mol, 82% yield) of a colorless solid are obtained.

1. temperaturethe reaction solution is cooled
2. customthe solvent is removed in vacuo
3. customThe resulting residue is purified by flash chromatography on silica gel (mobile phase: dichloromethane/methanol 50:1)