Reaktion #94268

ord-22d25771c50e412ea5e7d2f071eb77f4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe mixture is evaporated in vacuo
  3. 3
    workup.ADDITIONof chloroform are added
  4. 4
    ExtraktionAfter agitation, the chloroform extract
  5. 5
    Sonstigeis separated
  6. 6
    Trocknendried with Na2SO4
  7. 7
    SonstigeEvaporation
  8. 8
    Sonstigeyields an oily product which
  9. 9
    Sonstigeof 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151° ), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°

Vorschrift

14.6 g. of 4-chloro-2-methyl-6-phenyl-2H-pyrazolo [3,4-b]pyridine (0.06 mol.) and a solution of 100 ml. of methylpropylamine in 150 ml. of benzene are heated at 220° in an autoclave for 20 hours. After cooling, the mixture is evaporated in vacuo, and to the residue 100 ml. of water and 100 ml. of chloroform are added. After agitation, the chloroform extract is separated and dried with Na2SO4. Evaporation yields an oily product which, after treatment with ether, becomes solid. 14.3 g. of 2-methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]pyridin-4-amine, (m.p. 148°-151° ), are recrystallized from ethyl acetate giving a pure product of the melting point 156°-157°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04129738uspto-grants-1978_12