Reaktion #94270

ord-f4317951d12c45a6a95a5810ef649016

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is heated at 150° in an autoclave for 5 hours
  2. 2
    TemperaturAfter cooling
  3. 3
    Filtrationthe crystallized 4-ethoxy-2-methyl-6-phenyl2H-pyrazolo[3,4-b]pyridine is filtered off
  4. 4
    Waschenwashed with alcohol
  5. 5
    Sonstigeis obtained by evaporation of the mother liquor, total yield: 8.6 g
  6. 6
    SonstigeRecrystallization from ethanol
  7. 7
    Sonstigegives a product of the melting point 171°-172°

Vorschrift

8.5 g. of 4-chloro-2-methyl-6-phenyl-2H-pyrazolo[3,4-b]pyridine (0.035 mol.) are added to a solution of 0.9 g. of sodium (0.038 mol.) in 100 ml. of absolute ethanol. The mixture is heated at 150° in an autoclave for 5 hours. After cooling, the crystallized 4-ethoxy-2-methyl-6-phenyl2H-pyrazolo[3,4-b]pyridine is filtered off, washed with alcohol and then with water, yield: 6.2 g.; m.p. 170°-171°. An additional crop of 2.4 g. is obtained by evaporation of the mother liquor, total yield: 8.6 g. (97%). Recrystallization from ethanol gives a product of the melting point 171°-172°.

Quelle

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