Reaktion #8014

ord-9f4fc513dafa4ea6aad188ea8bbf6697

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Sonstigeto drop back to room temperature
  2. 2
    ExtraktionThe mixture was extracted with chloroform
  3. 3
    TrocknenThe extract was dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  5. 5
    Sonstigethe residue was purified by column chromatography on silica gel [chloroform/methanol (40/1)]

Vorschrift

To 6-(3-fluoro-4-methylphenyl)-2-isobutyl-4-methane-sulfonyloxymethyl-2H-pyridazin-3-one (100 mg, 0.27 mmol) was added a 40% aqueous dimethylamine (1 mL), and the mixture was stirred at 80° C. for 2 hours. The temperature of the reaction mixture was allowed to drop back to room temperature, and then, water was added. The mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel [chloroform/methanol (40/1)] to yield the title compound as a yellow oil (69.7 mg, 80.9%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087606B2uspto-grants-2006_08