Benzene → 2-Methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]-pyridin-4-amine

HRID 2071642Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2071642
Cl[C:2]1[C:3]2[C:4](=[N:14][N:15]([CH3:17])[CH:16]=2)[N:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:7]=1.C[NH:19][CH2:20][CH2:21][CH3:22].[CH:23]1C=CC=CC=1>CCOCC>[CH3:17][N:15]1[CH:16]=[C:3]2[C:4]([N:5]=[C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:7]=[C:2]2[NH:19][CH:20]([CH3:23])[CH2:21][CH3:22])=[N:14]1

Komponenten

5

Edukt 3

HCID 241BenzeneHCID 12315N-MethylpropylamineHCID 22756855HCID 22756855, Verbindung

Produkt 1

HCID 227568612-Methyl-N-(1-methylpropyl)-6-phenyl-2H-pyrazolo[3,4-b]-pyridin-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

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°.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe mixture is evaporated in vacuo
  3. additionof chloroform are added
  4. extractionAfter agitation, the chloroform extract
  5. customis separated
  6. dry with materialdried with Na2SO4
  7. customEvaporation
  8. customyields an oily product which
  9. customof 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°

Quellen und Nachweise

ORD-Eintrag
ord-5015d849e73641948321aeec7aa0aef8
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04048184

Notizen zur Reaktion

Wird geladen…