HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Nitrobenzaldehyde → Nicardipine Impurity 19
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Nitrobenzaldehyde | HCID 7449 | — |
| Edukt | Hexane | HCID 8058 | — |
| Edukt | Acetoacetate | HCID 6971017 | — |
| Edukt | 2-Cyanoethyl 3-aminocrotonate | HCID 13671410 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | Nicardipine Impurity 19 | HCID 10429284 | 78,2% |
Reaktionsschritte
9.7 g of 2-nitratoethyl acetoacetate, 7.7 g of 2-cyanoethyl 3-aminocrotonate and 7.6 g of 3-nitrobenzaldehyde in 76 ml of ethanol were heated at reflux for 7 hours. The mixture was treated in a manner similar to that of Referential Example 1, and the crystals thus obtained were applied to a silica gel column chromatography [eluent: a mixture of hexane and acetone (5:3)] and recrystallized from isopropyl alcohol to give 14.5 g of 2,6-dimethyl-4-(3-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 |
|---|---|
| Patentnummer | US04730052 |
| Quelldatensatz | uspto-grants-1988_03 |
| ORD ID | ord-0dca125cae514566a3d1d75fe4e31e20 |
| Quellennotiz | uspto-grants-1988_03 |