Reaktion #43354

ord-98a6e45d20c14bf48c3dda323bd78c88

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction liquid
  2. 2
    Waschenwashed with saturated brine
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    EinengenConcentrating the solvent under reduced pressure
  5. 5
    Sonstigethe residue was recrystallized
  6. 6
    workup.ADDITIONfrom mixed solvent of ethyl acetate and heptane

Vorschrift

5N aqueous hydrochloric acid (2.4 mL, 12 mmols) was added to THF (2.4 mL) solution of 1-(4-{2-[(3S)-3-{[tert-butyl(dimethyl)silyl]oxy}-1-pyrrolidinyl]ethoxy]phenyl}-4-[(5-chloro-2-pyridinyl)methoxy]-1H-pyridin-2-one (264.7 mg, 0.48 mmol), and stirred at room temperature for 2 hours. The reaction liquid was neutralized with 1N aqueous sodium hydroxide, extend with chloroform, washed with saturated brine and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the residue was recrystallized from mixed solvent of ethyl acetate and heptane, to provide the title compound (199.8 mg, 95%).

Quelle

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