反应详情

Suspend diethylacetamidomalonate (44 g, 0.203 mol), alpha-bromo-p-toluonitrile (40 g, 0.204 mol), potassium iodide (10 g) in dioxane (400 mL) and add a solution of sodium ethoxide (4.6 g of sodium in 200 mL of dry ethanol). Heat under reflux the mixture for 3-4 hours and let stay overnight. Pour the mixture on ice (2 L), filtrate the precipitate, wash with water and dry on lyophyliser. Recrystallize from methanol, to give diethyl 4-cyanobenzylacetamidomalonate as white crystals (61 g, 91%).

1. temperatureHeat
2. temperatureunder reflux the mixture for 3-4 hours
3. additionPour the mixture on ice (2 L), filtrate the precipitate
4. washwash with water
5. customdry on lyophyliser
6. customRecrystallize from methanol