Reaktion #67989

ord-550d0306c7964def8c9e5963eb868381

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Temperaturunder reflux
  3. 3
    Temperaturby heating
  4. 4
    SonstigeThe solvent was removed under reduced pressure, and water and ethyl acetate
  5. 5
    workup.ADDITIONwere added
  6. 6
    SonstigeThe organic layer was separated
  7. 7
    Extraktionthe aqueous layer was extracted with ethyl acetate
  8. 8
    Waschenthe resultant solution was washed with an aqueous saturated sodium chloride solution
  9. 9
    Trocknendried over anhydrous magnesium sulfate
  10. 10
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

To 30 mL of a xylene solution containing 2.3 g of methyl 3-oxo-3-(1,3-thiazol-2-yl)propionate, 1.4 mL of m-anisidine was added. The reaction mixture was stirred for 6 hours under reflux by heating. The solvent was removed under reduced pressure, and water and ethyl acetate were added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 3.3 g of a brown oily substance, N-(3-methoxyphenyl)-3-oxo-3-(1,3-thiazol-2-yl)propaneamide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524738B2uspto-grants-2013_09