تفاعل #9279

ord-b0d69462f11d46589ba57d6318c7fae0

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added 4 times at 30 minute intervals
  2. 2
    غسيلthe extract was washed with water and brine
  3. 3
    تجفيفAfter drying over anhydrous magnesium sulfate and filtration
  4. 4
    تركيزthe solvent was concentrated under reduced pressure
  5. 5
    أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

After dissolving 7-(2,4-dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine (280 mg) in acetonitrile (20 mL), nitronium tetrafluoroborate (255 mg) was added 4 times at 30 minute intervals while stirring on ice. The reaction mixture was added to ice water, extraction was performed with ethyl acetate and the extract was washed with water and brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (115 mg) was obtained from the n-hexane:ethyl acetate (20:1) fraction as yellow crystals.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091215B2uspto-grants-2006_08