HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate → Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate | HCID 40590 | — |
| Edukt | Acetoacetamide | HCID 80077 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate | HCID 13752508 | — |
Reaktionsschritte
Sodium acetate (30 g, 0.37 mol) is added to a stirred mixture of diethyl(ethoxymethylene)oxalacetate (87 g, 0.36 mol) and acetoacetamide (36 g, 0.36 mol) in absolute ethanol (300 mL). After stirring the reaction mixture for 30 minutes, the ethanol is distilled off under reduced pressure, the residue acidified to pH 2 with dilute aqueous hydrochloric acid and the resulting solid filtered off. Crystallization from an ethanol-water mixture affords diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate as crystals mp 200°-209° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04701208 |
| Quelldatensatz | uspto-grants-1987_10 |
| ORD ID | ord-11ec135ee81b486d86692e51990b1186 |
| Quellennotiz | uspto-grants-1987_10 |