HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Piperazine → 1-(4,6-Dimethylpyridin-2-YL)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Piperazine | HCID 4837 | — |
| Edukt | 2-Chloro-4,6-dimethylpyridine | HCID 12508378 | — |
| Lösungsmittel | Diglyme | HCID 8150 | — |
| Lösungsmittel | Sodium chloride; water | HCID 57417360 | — |
| Produkt | 1-(4,6-Dimethylpyridin-2-YL)piperazine | HCID 23368063 | 92,4% |
Reaktionsschritte
A solution of piperazine (195 g, 2.26 mol) in diglyme (250 mL) was heated to 160° C. and a solution of 2-chloro-4,6-dimethylpyridine (40 g, 0.283 mol) in diglyme (150 mL) was added over a period of 30 min. The mixture was maintained at this temperature for 36 hand then the reaction mixture was allowed to cool to ambient temperature, diluted with brine and extracted with ethyl acetate (3×500 mL). The combined organic layers were washed with brine (2×100 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to give the crude compound. Vacuum distillation to remove diglyme afforded 1-(4,6-dimethyl-2-pyridyl)piperazine (50 g, 92%) as an oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08993574B2 |
| Quelldatensatz | uspto-grants-2015_03 |
| ORD ID | ord-db10b6d3cbbd4a678c3bfb0ef46b2db1 |
| Quellennotiz | uspto-grants-2015_03 |