HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pyrrolidine → HCID 136463775, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pyrrolidine | HCID 31268 | — |
| Edukt | O-tert-butylhydroxylamine hydrochloride | HCID 2777906 | — |
| Edukt | 2-(5-Bromo-2-hydroxybenzoyl)-3-(1,3-dioxolan-2-yl)pyridine | HCID 19701635 | — |
| Lösungsmittel | 1-Propanol | HCID 1031 | — |
| Produkt | HCID 136463775 | HCID 136463775 | 80% |
Reaktionsschritte
A solution of 2-(5-bromo-2-hydroxybenzoyl)-3-(1,3-dioxolan-2-yl)pyridine (2.92 g), O-t-butyl-hydroxylamine hydrochloride (2.09 g) and pyrrolidine (1.78 g) in n-propanol (40 ml) was heated for 2 hours under reflux. The reaction mixture was concentrated, to which was added water, followed by subjecting the mixture to extraction with ethyl acetate. The extract solution was washed with a saturated aqueous saline solution, dried (anhydrous sodium sulfate), and concentrated. The concentrate was purified by means of a silica gel column chromatography (eluent: ethyl acetate/hexane) to give (Z)-2-(5-bromo-2-hydroxybenzoyl)-3-(1,3-dioxolan-2-yl)pyridine O-t-butyloxime (2.81 g) (Compound 134).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05716971 |
| Quelldatensatz | uspto-grants-1998_02 |
| ORD ID | ord-a0acd65784ad4ce680a9cb519443478b |
| Quellennotiz | uspto-grants-1998_02 |