HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus oxychloride → Benzonitrile, 4-(5,6,7,8-tetrahydroimidazo(1,5-a)pyridin-5-yl)-, hydrochloride (1:1)
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 4-(5,6,7,8-Tetrahydroimidazo[1,5-a]pyridin-5-yl)benzamide | HCID 13688221 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | Benzonitrile, 4-(5,6,7,8-tetrahydroimidazo(1,5-a)pyridin-5-yl)-, hydrochloride (1:1) | HCID 59694 | — |
Reaktionsschritte
A solution of 1.13 g of 5-(p-carbamoylphenyl)-5,6,7,8-tetrahydroimidazo[1,5-a]pyridine and 1.0 ml of phosphorus oxychloride in 30 ml of chloroform is refluxed for 15 h, cooled and evaporated with toluene. The resulting oil is redissolved in 30 ml of methylene chloride, cooled to 0° and 30 ml of an ice-cold solution of 50% ammonium hydroxide solution is added. The organic phase is separated, dried and evaporated to an oil. Filtration through 20 g of silica with ethyl acetate yields the free title compound which is dissolved in 20 ml of acetone and treated with 1.2 ml of 3N ethereal hydrogen chloride to yield its hydrochloride, m.p. 209°-210°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05428160 |
| Quelldatensatz | uspto-grants-1995_06 |
| ORD ID | ord-dfd00680e8a7424db1bb29c063bb5462 |
| Quellennotiz | uspto-grants-1995_06 |