HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus pentachloride → 4'-Chloro-2,2':6',2''-terpyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus pentachloride | HCID 24819 | — |
| Edukt | 2,6-Bis(2-pyridyl)-4(1H)-pyridone | HCID 619353 | — |
| Lösungsmittel | Phosphorus oxychloride | HCID 24813 | — |
| Produkt | 4'-Chloro-2,2':6',2''-terpyridine | HCID 667748 | — |
Reaktionsschritte
A mixture of 3.99 g (16 mmol) of 1′H-[2,2′;6′,2″]terpyridin-4′-one (L1) and 8.0 g (38 mmol) of phosphorus pentachloride is boiled at reflux in 200 ml of phosphorus oxychloride for sixteen hours. The mixture is allowed to cool and concentrated to dryness. 200 ml of ice-water are then added cautiously to the residue, and the solution is then adjusted to pH 9 with aqueous potassium hydroxide solution. Extraction is carried out three times using chloroform and the organic extracts are dried over sodium sulfate, filtered and concentrated. After recrystallisation from ethanol, 4′-chloro-[2,2′;6′,2″]terpyridine is obtained in the form of white needles.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07456285B2 |
| Quelldatensatz | uspto-grants-2008_11 |
| ORD ID | ord-f42e84c5a7db4dbd82af8fad9fdc2883 |
| Quellennotiz | uspto-grants-2008_11 |