Reaktion #68513

ord-d95bd4d1ba5843d38255cf8f6ae40564

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated under vacuum
  2. 2
    workup.DISSOLUTIONThe remaining residue was dissolved in ethyl acetate
  3. 3
    Waschenthen washed with water and brine
  4. 4
    ExtraktionThe aqueous layer was back-extracted with ethyl acetate (3×)
  5. 5
    Trocknendried over sodium sulfate
  6. 6
    Einengenthen concentrated under vacuum

Vorschrift

5-Bromopyridin-2(1H)-one (0.250 g, 1.44 mmol) was dissolved in DMF (3 mL) then added iodomethane (0.0943 ml, 1.51 mmol) and potassium carbonate (0.218 g, 1.58 mmol). The reaction was stirred at room temperature overnight. The reaction mixture was concentrated under vacuum. The remaining residue was dissolved in ethyl acetate then washed with water and brine. The aqueous layer was back-extracted with ethyl acetate (3×). The organic layers were combined and dried over sodium sulfate then concentrated under vacuum to afford 5-bromo-1-methylpyridin-2(1H)-one as an orange waxy solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524900B2uspto-grants-2013_09