Reaktion #426736

ord-7b3f524f606a4c85802e103451f69231

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 17 h
  3. 3
    Temperaturto cool
  4. 4
    Temperaturheating
  5. 5
    Sonstigethe solvent was removed under reduced pressure
  6. 6
    Sonstigethe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08895313B2uspto-grants-2014_11