Reaktion #1765251

ord-745569c5209447429626f19e87c6d2d6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture was heated
  2. 2
    Temperaturunder reflux for eighteen hours
  3. 3
    EinengenThe solution was concentrated to fifty percent
  4. 4
    workup.ADDITIONdiluted with water (100 mL)
  5. 5
    Extraktionextracted with ethyl acetate (2×100 mL)
  6. 6
    WaschenThe combined extracts were washed with brine
  7. 7
    Trocknendried (Na2SO4)
  8. 8
    Einengenconcentrated

Vorschrift

Sodium methoxide (2.8 g, 50 mmol) was added to a solution of 1-(6-chloro-pyridin-3-yl)-propan-1-one (2.8 g, 16.5 mmol) in methanol (70 mL) and the reaction mixture was heated under reflux for eighteen hours. The solution was concentrated to fifty percent, diluted with water (100 mL) and extracted with ethyl acetate (2×100 mL). The combined extracts were washed with brine, dried (Na2SO4) and concentrated to give product as a colorless oil (2.1 g, 77 percent yield), which was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08008487B2uspto-grants-2011_08