HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → 2-(4-[4-Methoxyphenyl]piperazin-1-yl)-5-phenoxycarbonylaminopyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Phenyl chloroformate | HCID 15891 | — |
| Edukt | 5-Amino-2-(4-[4-methoxyphenyl]piperazin-1-yl)pyridine | HCID 9161650 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-(4-[4-Methoxyphenyl]piperazin-1-yl)-5-phenoxycarbonylaminopyridine | HCID 14986889 | — |
Reaktionsschritte
To a mixture of the product of part (ii) (1.2 g, 4.2 mmole) and triethylamine (0.5 g, 5 mmole) in methylene chloride (20 ml) was added, dropwise, phenyl chloroformate (0.8 g, 5.1 mmole) and the resulting mixture was stirred at room temperature for 20 hours. The reaction was quenched by the addition of water, the aqueous phase separated and re-extracted with methylene chloride. The combined organic extracts were washed with aqueous sodium bicarbonate solution then water, dried over magnesium sulphate and concentrated under reduced pressure to provide a solid. Trituration of this solid material with ethanol yielded the desired product, m.p. 197°-198° (1.4 g, 83%), which was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05023258 |
| Quelldatensatz | uspto-grants-1991_06 |
| ORD ID | ord-f888aa0daee24a2495c91f58190ffbdc |
| Quellennotiz | uspto-grants-1991_06 |