HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → 2,4-Dimethyl-4,5-dihydro[3,4'-bipyridin]-6(1H)-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 4-Acetyl-3-methyl-4-(4-pyridinyl)butanenitrile | HCID 13268971 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 2,4-Dimethyl-4,5-dihydro[3,4'-bipyridin]-6(1H)-one | HCID 13268972 | — |
Reaktionsschritte
To a 2.0 g portion of 4-acetyl-3-methyl-4-(4-pyridinyl)butanenitrile dissolved in 20 ml of acetic acid was added dropwise 3 ml of sulfuric acid whereupon an exothermic reaction ensued. The reaction mixture was stirred for 4 hours, the acetic acid was evaporated off in vacuo and to the remaining material was added 10 ml of water followed by basification with 35% aqueous sodium hydroxide solution. The alkaline solution was extracted four times with ethyl acetate; the combined extracts were dried over anhydrous magnesium sulfate; the ethyl acetate was distilled off in vacuo; and, the remaining white solid was recrystallized from acetonitrile to produce 2.0 g of 3,4-dihydro-4,6-dimethyl-5-(4-pyridinyl)-2(1H)-pyridinone, m.p. 184°-186° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04431651 |
| Quelldatensatz | uspto-grants-1984_02 |
| ORD ID | ord-93e400e519c24881b0c6065f83559ef3 |
| Quellennotiz | uspto-grants-1984_02 |