Reaktion #94268
ord-22d25771c50e412ea5e7d2f071eb77f4
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling
- 2Sonstigethe mixture is evaporated in vacuo
- 3workup.ADDITIONof chloroform are added
- 4ExtraktionAfter agitation, the chloroform extract
- 5Sonstigeis separated
- 6Trocknendried with Na2SO4
- 7SonstigeEvaporation
- 8Sonstigeyields an oily product which
- 9Sonstigeof 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°.