反応 #53756

反応方程式

ethyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy)acetoacetate

ethyl-3-aminocrotonate

→

Diethyl 4-(2-chlorophenyl)-2-{[2-(1,3-dioxo-1.3-dihydro-2H-isoindol-2-yl)ethoxy]methyl}-6-methyl-1.4-dihydro-3.5-pyridine dicarboxylate

溶媒

2-propanol

反応条件

後処理

1. 1
   温度the mixture was heated at the same temperature for 16 hours
2. 2
   その他The mixture was evaporated to dryness
3. 3
   workup.DISSOLUTIONThe residue was dissolved in 180 ml of glacial acetic acid at 80° C
4. 4
   ろ過The solid was filtered off
5. 5
   洗浄washed with 92 ml of glacial acetic acid
6. 6
   workup.DISSOLUTIONThe solid was dissolved in 75 ml of ethanol at 80° C
7. 7
   温度The solution was cooled to 20° C.
8. 8
   workup.STIRRINGthe suspension was agitated for 2 h
9. 9
   ろ過The solid was filtered off
10. 10
    洗浄washed with 25 ml of ethanol
11. 11
    その他The wet product was recrystallized from 60 ml of ethyl acetate

実験手順

116.7 g of ethyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy)acetoacetate was dissolved in 120 ml of 2-propanol at 80° C. 31.2 g of ethyl-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 180 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 92 ml of glacial acetic acid. The solid was dissolved in 75 ml of ethanol at 80° C. The solution was cooled to 20° C. and the suspension was agitated for 2 h. The solid was filtered off, washed with 25 ml of ethanol. The wet product was recrystallized from 60 ml of ethyl acetate.

出典