反应详情

温度

110 °C

At room temperature, a solution of 37.2 ml (267 mmol) of triethylamine and 7.6 ml (202 mmol) of formic acid in 100 ml of dioxane is added to a solution of 40 g (80.9 mmol) of diallyl 2-[4-(methoxycarbonyl)benzyl]-2-{2-[4-(methoxycarbonyl)phenyl]ethyl}malonate, 1.49 g (5.67 mmol) of triphenylphosphine and 363 mg of palladium acetate in 500 ml of dioxane. The reaction mixture is then stirred at 110° C. overnight. After the reaction has gone to completion, the reaction solution is cooled and the solvent is removed under reduced pressure. The residue obtained is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1). This gives 20.98 g (56.6 mmol, 70% of theory) of a colorless solid.

1. temperaturethe reaction solution is cooled
2. customthe solvent is removed under reduced pressure
3. customThe residue obtained
4. customis purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 4:1)