反応 #4756

反応方程式

2-(4-chlorobutoxy)-5-nitrobenzaldehyde

ethyl propionylacetate

piperidine

acetic acid

benzene

→

diethyl 2-ethyl-4-[2-(4-chlorobutoxy)-5-nitrophenyl]-6-methyl-1,4-dihydropyridine-3,5-dicarboxylate

反応条件

後処理

1. 1
   温度the solution was refluxed for 9 hours
2. 2
   その他while removing water using a Dean-Stark trap
3. 3
   温度After cooling the reaction solution, 6.52 g of ethyl 3-aminocrotonate
4. 4
   workup.ADDITIONwas added to the solution
5. 5
   温度the mixture was refluxed
6. 6
   温度under heating for 11 hours
7. 7
   温度After cooling the mixture
8. 8
   その他precipitated crude crystals
9. 9
   ろ過were collected by filtration
10. 10
    その他recrystallized from methanol

実験手順

In 106 ml of dry benzene were dissolved 13.0 g of 2-(4-chlorobutoxy)-5-nitrobenzaldehyde, 7.28 g of ethyl propionylacetate, 0.20 ml of piperidine and 0.62 ml of acetic acid, and the solution was refluxed for 9 hours while removing water using a Dean-Stark trap. After cooling the reaction solution, 6.52 g of ethyl 3-aminocrotonate was added to the solution, and the mixture was refluxed under heating for 11 hours. After cooling the mixture, precipitated crude crystals were collected by filtration, and recrystallized from methanol to give 13.13 g of diethyl 2-ethyl-4-[2-(4-chlorobutoxy)-5-nitrophenyl]-6-methyl-1,4-dihydropyridine-3,5-dicarboxylate.

出典