Reaktion #1269089

ord-b638464ecdc94b1aa16e4e818278bd43

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  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
    Waschenwashed with water
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07285666B2uspto-grants-2007_10