Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-Nitrobenzaldehyde | HCID 11101 | — |
| Edukt | Acetoacetate | HCID 6971017 | — |
| Edukt | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| Katalysator | Piperidine | HCID 8082 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | HCID 86742032 | HCID 86742032 | 77,1% |
Reaktionsschritte
9.7 g of 2-nitratoethyl acetoacetate, 7.6 g of 2-nitrobenzaldehyde and 0.2 g of piperidine in 40 ml of benzene were heated at reflux under azeotropic dehydration conditions for 3 hours. The mixture was treated in a manner similar to that of Referential Example 1, there was obtained the residue, to which was added 7.7 g of 2-cyanoethyl 3-aminocrotonate. The mixture was taken up in 40 ml of isopropyl alcohol and heated at reflux for 3 hours. The isopropyl alcohol was evaporated under reduced pressure, and the residue was applied to a silica gel column chromatography (eluent: dichromomethane) and recrystallized from a mixture of dichromethane and diethyl ether to give 14.3 g of 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-cyanoethyl) ester 5-(2-nitratoethyl) ester.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04730052 |
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| Quelldatensatz | uspto-grants-1988_03 |
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| ORD ID | ord-4cf9e1f8e25540d2adad8a7c7a6e113c |
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| Quellennotiz | uspto-grants-1988_03 |
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