HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diphenyl Ether → HCID 178469631, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diphenyl Ether | HCID 7583 | — |
| Edukt | Diethyl {[(1-ethyl-1H-pyrazol-5-yl)amino]methylene}malonate | HCID 12845080 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178469631 | HCID 178469631 | — |
Reaktionsschritte
253 g. of [[(1-Ethyl-5-pyrazolyl)amino]methylene]malonic acid diethyl ester (0.09 mol.) are dissolved in 770 g. of diphenyl ether. The reaction mixture is heated to 235°-250° (bath temperature) and allowed to react at this temperature for 1-2 hours while the resulting ethanol is continuously distilled off. The last amount of alcohol is removed by means of a water aspirator. The diphenyl ether is separated by distillation with a fractionating column in vacuo. The 1-ethyl-4-hydroxy-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid ethyl ester is obtained at b.p.0.05 115°-120°, yield 195 g.= 92% of theory, m.p. 85°-87°. The compound is recrystallized from benzene (90° to 100°), m.p. 87°-89°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04012373 |
| Quelldatensatz | uspto-grants-1977_03 |
| ORD ID | ord-a611a73573d54e3abb63d3cfb1640ad8 |
| Quellennotiz | uspto-grants-1977_03 |