반응 #9300

ord-605836c3183744a0b6fa01960338a1b7

반응 조건

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

후처리

  1. 1
    여과The reaction mixture was filtered with celite
  2. 2
    농축the obtained filtrate was concentrated under reduced pressure
  3. 3
    workup.ADDITIONWater was added
  4. 4
    추출extraction
  5. 5
    세척the extract was washed with saturated aqueous sodium hydrogencarbonate and brine
  6. 6
    건조dried over magnesium sulfate
  7. 7
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

2-Ethyl-4-methoxy-7-(2-methoxy-4,6-dimethylphenyl)-3-nitropyrazolo[1,5-a]pyridine (185 mg) was dissolved in a mixture of ethanol (7 mL) and water (7.5 mL), and then acetic acid (0.3 mL) and zinc powder (185 mg) were added and the reaction mixture was heated at 60° C. for 20 minutes. The reaction mixture was filtered with celite, and the obtained filtrate was concentrated under reduced pressure. Water was added, 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 to obtain 2-ethyl-4-methoxy-7-(2-methoxy-4,6-dimethylphenyl)pyrazolo[1,5-a]pyridin-3-amine as a crude product.

출처

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