反应详情

温度

15 °C

350 g of crude ethyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy) acetoacetate from Example 1 was dissolved in 540 ml of 2-propanol at 80° C. 50 g of methyl-3-aminocrotonate was added and the mixture was heated at the same temperature for 16 hours. The mixture was evaporated to dryness. The residue was dissolved in 540 ml of glacial acetic acid at 80° C. The mixture was cooled to 15° C. and stirred at the same temperature for 20 hours. The formed solid was filtered off and washed with 280 ml of glacial acetic acid. The solid was suspended in 225 ml of methanol and agitated for 30 minutes. The solid was filtered off, washed with 75 ml of methanol and dried.

1. temperaturethe mixture was heated at the same temperature for 16 hours
2. customThe mixture was evaporated to dryness
3. dissolutionThe residue was dissolved in 540 ml of glacial acetic acid at 80° C
4. filtrationThe formed solid was filtered off
5. washwashed with 280 ml of glacial acetic acid
6. stirringagitated for 30 minutes
7. filtrationThe solid was filtered off
8. washwashed with 75 ml of methanol
9. customdried