HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde oxime
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Hydroxyamine hydrochloride | HCID 443297 | — |
| Edukt | 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde | HCID 45480192 | — |
| Lösungsmittel | Methanol--water (1/1) | HCID 22242641 | — |
| Produkt | 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde oxime | HCID 131736879 | 97,8% |
Reaktionsschritte
To a solution of 5-bromo-2-fluoro-pyridine-3-carbaldehyde (2) (20.0 g, 98.0 mmol) in 1:1 MeOH—H2O (250 mL) was added hydroxylamine hydrochloride (7.52 g, 108 mmol) and sodium carbonate (11.4 g, 108 mmol). The reaction mixture was stirred at rt for 1 hour. The solvent was evaporated in vacuo and the residue diluted with H2O (200 mL) and EtOAc (200 mL). The organic phase was separated, dried (Na2SO4), filtered and the solvent evaporated in vacuo. The product was obtained as a light pink solid (21.0 g, 93%); Rf: 0.4 (10% EtOAc-pet ether).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09433622B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-e1b82a2e6c5043789b778fa207d56113 |
| Quellennotiz | uspto-grants-2016_09 |