반응 #9326

ord-a6c0895ec1c047d8b96e9207f20ccfd8

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.DISTILLATIONwas distilled off under reduced pressure
  3. 3
    workup.ADDITIONsaturated aqueous sodium hydrogencarbonate and ethyl acetate were added to the residue and extraction
  4. 4
    세척washed with water
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

After dissolving 7-(2,6-dimethoxy-4-methylphenyl)-2-ethyl-3-nitropyrazolo[1,5-a]pyridine (600 mg) in a mixture of ethanol (30 mL) and water (30 mL), acetic acid (3 mL) and zinc powder (600 mg) were added and the mixture was stirred at 60° C. for 2 hours. The ethanol of the obtained reaction mixture was distilled off under reduced pressure, and then saturated aqueous sodium hydrogencarbonate and ethyl acetate were added to the residue and extraction was performed with ethyl acetate. The obtained organic layers were combined, washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 7-(2,6-dimethoxy-4-methylphenyl)-2-ethylpyrazolo[1,5-a]pyridine-3-amine (500 mg) as a crude product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091215B2uspto-grants-2006_08