Reaktion #426736
ord-7b3f524f606a4c85802e103451f69231
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturunder reflux for 17 h
- 3Temperaturto cool
- 4Temperaturheating
- 5Sonstigethe solvent was removed under reduced pressure
- 6Sonstigethe residue was purified by flash chromatography (1:1 Hexane/EtOAc)
Vorschrift
A mixture of 2-amino-5-picoline (0.88 g, 8.19 mmol) and 2-bromo-4′-nitroacetophenone (2.0 g, 8.19 mmol) in EtOH (50 ml) was heated under reflux for 17 h. The reaction mixture was allowed to cool and sodium bicarbonate (840 mg, 9.99 mmol) was added and heating was continued for 18 h. On cooling to room temperature, the solvent was removed under reduced pressure and the residue was purified by flash chromatography (1:1 Hexane/EtOAc) to give the title compound (0.84 g, 40%) as a yellow solid.