Reaktion #43333

ord-f177d71729334e70bce27de2868c1f16

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenby washing with water and saturated brine
  2. 2
    Trocknendrying over anhydrous sodium sulfate
  3. 3
    EinengenConcentrating
  4. 4
    Sonstigethe reaction liquid under reduced pressure
  5. 5
    Sonstigethe residue was purified on silica gel column chromatography (C-300; methanol:chloroform=1:20-1:10)

Vorschrift

Potassium carbonate (11 mg, 0.08 mmol) and methyl p-toluenesulfonate (6 mg, 0.03 mmol) were added to DMF (2 mL) solution of 4-[(E)-2-4-hydroxyphenyl)vinyl]-1-{4-[2-(1-pyrrolidinyl)ethoxy]phenyl}-1H-pyridin-2-one (11 mg, 0.03 mmol), and stirred for a day and night at 80° C. Ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine and drying over anhydrous sodium sulfate. Concentrating the reaction liquid under reduced pressure, the residue was purified on silica gel column chromatography (C-300; methanol:chloroform=1:20-1:10) to provide the title compound (6 mg, 53%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732456B2uspto-grants-2010_06