HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Piperazine → 1-(3-Nitropyridin-2-yl)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Piperazine | HCID 4837 | — |
| Edukt | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 1-(3-Nitropyridin-2-yl)piperazine | HCID 3778834 | — |
Reaktionsschritte
A solution of 2-chloro-3-nitropyridine (4.76 g, 30 mmol) and piperazine (5.9, 69 mmol) in acetonitrile, (75 mL), was stirred at reflux for 5 h. After concentrating under reduced pressure, the residue was partitioned between ethyl acetate and 10% NaOH. The ethyl acetate extract was washed with water, dried (Na2SO4), filtered and concentrated. Flash chromatography over Al2O3 and elution with 2% MeOH-98% CHCl3 afforded the title compound, m.p. 82°-87° C. An analytical sample, m.p. 83.5°-86.5° C., was obtained upon recrystallization from CHCl3 -hexane.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04442103 |
| Quelldatensatz | uspto-grants-1984_04 |
| ORD ID | ord-354e584d27204713935bafa4bda00ee9 |
| Quellennotiz | uspto-grants-1984_04 |