Hydrochloric Acid → HCID 86606798, Verbindung

HRID 42595Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 42595
C([O:3][CH:4](OCC)[CH2:5][N:6]1[CH:14]=[C:13]2[C:8]([N:9]=[C:10]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[C:11]([C:22]3[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=3)=[C:12]2[C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)=[N:7]1)C.Cl>>[F:21][C:18]1[CH:19]=[CH:20][C:15]([C:12]2[C:13]3[C:8](=[N:7][N:6]([CH2:5][CH:4]=[O:3])[CH:14]=3)[N:9]=[C:10]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[C:11]=2[C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)=[CH:16][CH:17]=1

Komponenten

3

Edukt 2

HCID 313Hydrochloric AcidHCID 684434952-(2,2-Diethoxyethyl)-4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridine

Produkt 1

HCID 86606798HCID 86606798, VerbindungAusbeute 65 %

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

In a volumetric flask, 2-(2,2-diethoxyethyl)-4,6-bis(4-fluorophenyl)-5-(4-pyridyl)pyrazolo[3,4-b]pyridine (0.31 g, 0.6 mmol, obtained in example 73) and 1 N HCl (2.6 mL) were introduced. The mixture was heated to 100° C. for 1 hour. It was allowed to cool, adjusted to pH=7 and extracted with EtOAc. The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity eluent, to afford 166 mg of the title compound (yield: 65%).

Aufarbeitung

  1. temperatureto cool
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated to dryness
  5. customThe crude product obtained
  6. customwas purified by chromatography on silica gel
  7. temperatureof increasing polarity eluent

Quellen und Nachweise

ORD-Eintrag
ord-a816b7e7d0d5449ab9764d09d3403a06
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08536194B2

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