Reaktion #9320

ord-0073396e34064309a3a1966475a4eabd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe extract was washed with saturated aqueous sodium hydrogencarbonate and brine
  2. 2
    Trocknendried over magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Vorschrift

m-Chloroperbenzoic acid (91 mg) was added to a solution of N,N-dicyclopropylmethyl-N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfinyl)pyrazolo[1,5-a]pyridin-3-yl]amine (162 mg) in dichloromethane (10 mL) at 0° C., and the mixture was stirred for 4 hours. Water was added to the reaction mixture, extraction was performed with ethyl acetate, the extract was washed with saturated aqueous sodium hydrogencarbonate and brine and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (10 g), and the title compound (9 mg) was obtained from the n-hexane:ethyl acetate (1:2) fraction as a yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091215B2uspto-grants-2006_08