تفاعل #9280

ord-9dbfc3c4f4ce448e87c72ec2f1ff0d08

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    workup.STIRRINGstirring
  3. 3
    غسيلthe extract was washed with water and brine
  4. 4
    تجفيفAfter drying over anhydrous magnesium sulfate and filtration
  5. 5
    تركيزthe solvent was concentrated under reduced pressure
  6. 6
    أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

After dissolving 7-bromo-2-ethylpyrazolo[1,5-a]pyridine (1.1 g) in acetonitrile (20 mL), nitronium tetrafluoroborate (1.3 g) was added while stirring on ice, and stirring was continued for 30 minutes. 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 (670 mg) was obtained from the n-hexane:ethyl acetate (10:1) fraction as yellow crystals.

المصدر

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