HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzonitrile → 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-A]pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzonitrile | HCID 7505 | — |
| Edukt | 1,10-Phenanthroline hydrate | HCID 21226 | — |
| Edukt | 2-Amino-4-bromopyridine | HCID 693282 | — |
| Katalysator | copper(I) bromide | HCID 24593 | — |
| Produkt | 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-A]pyridine | HCID 67775500 | 72% |
Reaktionsbedingungen
| Temperatur | 130 °C |
|---|
Reaktionsschritte
A mixture of 2-amino-4-bromopyridine (5.00 g, 28.9 mmol), copper (I) bromide (207 mg, 1.44 mmol), 1,10-phenanthroline monohydrate (289 mg, 1.44 mmol) and benzonitrile (40 mL) was heated in a 100-mL 4-necked flask to 130° C. During 23 h a gentle flow of air was bubbled through the reaction mixture (91% conversion, HPLC method cf. example 1.3). The dark brown suspension was then cooled to 0-5° C. and filtered. The filter cake was washed with TBME (50 mL) and dried to yield crude 7-bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine (6.39 g, 72%) as a green solid with 89.4% purity (HPLC area-%, HPLC method cf. example 1.3).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09115130B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-de7cd88362d84a54bd9b4fc87953dff8 |
| Quellennotiz | uspto-grants-2015_08 |