반응 #4756

반응 방정식

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

반응 조건

후처리

1. 1
   온도the solution was refluxed for 9 hours
2. 2
   기타while removing water using a Dean-Stark trap
3. 3
   온도After cooling the reaction solution, 6.52 g of ethyl 3-aminocrotonate
4. 4
   workup.ADDITIONwas added to the solution
5. 5
   온도the mixture was refluxed
6. 6
   온도under heating for 11 hours
7. 7
   온도After cooling the mixture
8. 8
   기타precipitated crude crystals
9. 9
   여과were collected by filtration
10. 10
    기타recrystallized from methanol

실험 절차

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.

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