Reaktion #1354448

ord-084482090a4f4d888f59b0fc40d0a938

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe solvent was concentrated under a reduced pressure
  2. 2
    workup.ADDITIONthe residual oily matter was mixed with saturated sodium bicarbonate aqueous solution
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with saturated brine
  5. 5
    Trocknendried with magnesium sulfate
  6. 6
    Sonstigethe solvent was evaporated under a reduced pressure
  7. 7
    SonstigeThereafter, the thus obtained mixture was purified by a silica gel column chromatography (ethyl acetate:hexane 1:1)

Vorschrift

A 500 mg portion of pyridine-4-aldehyde was dissolved in 15 ml of acetic acid, and the solution was mixed with 509 mg of o-aminophenol and stirred with heating at 100° C. for 6 hours. The solvent was concentrated under a reduced pressure, and the residual oily matter was mixed with saturated sodium bicarbonate aqueous solution and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate, and then the solvent was evaporated under a reduced pressure. Thereafter, the thus obtained mixture was purified by a silica gel column chromatography (ethyl acetate:hexane 1:1) to obtain the title compound (90 mg) in light yellow color.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06552057B2uspto-grants-2003_04