Methyl 3-aminocrotonate → 4-(2-Chlorophenyl)-2-[[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethoxy]methyl]-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylic Acid 3,5-Dimethyl Ester

92.1 g of methyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy)acetoacetate was dissolved in 108 ml of 2-propanol at 80° C. 31.3 g of methyl-3-aminocrotonate was added and the mixture was heated at the same temperature for 24 hours. The mixture was evaporated to dryness. The residue was dissolved in 162 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 solid was filtered off and washed with 83 ml of glacial acetic acid. The solid was suspended in 68 ml of methanol and agitated for 30 minutes. The solid was filtered off, washed with 23 ml of methanol and dried. The product was recrystallized from ethyl acetate.

1. temperaturethe mixture was heated at the same temperature for 24 hours
2. customThe mixture was evaporated to dryness
3. dissolutionThe residue was dissolved in 162 ml of glacial acetic acid at 80° C
4. filtrationThe solid was filtered off
5. washwashed with 83 ml of glacial acetic acid
6. stirringagitated for 30 minutes
7. filtrationThe solid was filtered off
8. washwashed with 23 ml of methanol
9. customdried
10. customThe product was recrystallized from ethyl acetate

ORD 기록

ord-37af752ca5b5457c9f1e81b7de7d9e72

출처 데이터셋

uspto-grants-2005_02

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06858738B2