HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 5-Nitro-2-(2-cyanoethyl)-3-methylpyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 3-(3-Methyl-5-nitropyrid-2-yl)-3,3-bis(carbethoxy)propionitrile | HCID 19851796 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 5-Nitro-2-(2-cyanoethyl)-3-methylpyridine | HCID 19851777 | 61,4% |
Reaktionsschritte
3-(3-Methyl-5-nitropyrid-2-yl)-3,3-bis(carbethoxy)propionitrile (29.8 g) was dissolved in methanol (1120 ml), molar sodium hydroxide solution (355 ml) was added, the reaction was cooled from 28° C. to room temperature and stirred for 55 minutes. The pH was lowered to 4 by the addition of concentrated hydrochloric acid, the reaction was stirred for 2.75 hr., the pH was then raised to 7 and the methanol was distilled off. The aqueous phase was extracted with chloroform, extracts were dried, filtered and concentrated. The residue was crystallised from chloroform/petroleum ether 40°-60° C. The crude product was treated with charcoal in ethanol and recrystallised from ethanol to give the title compound 10.44 g, m.p. 73°-74° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04764519 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-53d7ad8220734ff5868589de7ff6ea4e |
| Quellennotiz | uspto-grants-1988_08 |