반응 #9280

반응 방정식

ethyl acetate

7-bromo-2-ethylpyrazolo[1,5-a]pyridine

nitronium tetrafluoroborate

→

title compound

수율 50.8%

7-Bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine

수율 50.8%

용매

acetonitrile

반응 조건

후처리

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

실험 절차

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.

출처