HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Nitrobenzaldehyde → Nicardipine Impurity 19
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Nitrobenzaldehyde | HCID 7449 | — |
| Edukt | Acetoacetate | HCID 6971017 | — |
| Edukt | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | Nicardipine Impurity 19 | HCID 10429284 | 88,4% |
Reaktionsschritte
10.3 g of 3-nitratopropyl acetoacetate, 7.7 g of 2-cyanoethyl 3-aminocrotonate and 7.6 g of 3-nitrobenzaldehyde in 76 ml of isopropyl alcohol were heated at reflux for 6.5 hours, and cooled on ice. The crystals which precipitated were collected by filtration, dried, applied to a silica gel column chromatography (eluent: dichloromethane) and recrystallized from ethanol to give 16.4 g of 2,6-dimethyl-4-(3-nitrophenyl)1,4-dihydropyridine-3,5-dicarboxylic acid 3-(2-cyanoethyl) ester 5-(3-nitratopropyl) ester.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04730052 |
| Quelldatensatz | uspto-grants-1988_03 |
| ORD ID | ord-cf05da0d5c2c4a7cb1ab8b92df4a8cd5 |
| Quellennotiz | uspto-grants-1988_03 |