反应详情

温度

-10 °C

188 g (1 mol) of diisopropyl malonate, 571 g (3 mol) of triisopropyl orthoformate and 0.05 g of catalyst from Example 5 were initially introduced into the apparatus mentioned in Example 1 and the mixture was heated to -10° C. 102 g of acetic anhydride were then metered in over the course of 5 hours. The bottom temperature was raised to 150° C. At the same time a low-boiling fraction was removed under reflux at a boiling temperature of 60° C. After 10 hours, the formation of low-boiling component decreased. The mixture was then fractionated in vacuo, first at 15 mbar and then at 0.3 mbar. 7.6% of diisopropyl malonate, 80.2% of diisopropyl isopropoxymethylenemalonate and 6.5% of diisopropyl diisopropoxy-methylmalonate were obtained. The last-mentioned compound was converted into diisopropyl isopropoxymethylenemalonate by heating with 0.2 g of H3PO4.

1. customwere then metered in over the course of 5 hours
2. temperatureThe bottom temperature was raised to 150° C
3. customAt the same time a low-boiling fraction was removed
4. temperatureunder reflux at a boiling temperature of 60° C