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Potassium Carbonate → HCID 21894750, Verbindung

HRID 909147
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 909147
C([O-])([O-])=O.[K+].[K+].[Br:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[NH:13][N:12]=[CH:11]2>CN(C=O)C>[Br:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([CH2:9][CH:10]([CH3:14])[CH3:11])[N:12]=[CH:11]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 7619295-bromo-1H-indazole2×

Produkt 1

HCID 21894750HCID 21894750, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
105 °C

Versuchsvorschrift

K2CO3 was added to a solution of 5-bromoindazole and in DMF. The mixture was heated to 105° C. After disappearance of 5-bromoindazole the reaction mixture was poured onto DCM/brine. The two layers were separated and the aqueous layer was extracted with DCM (2×) and checked by TLC. The combined organics were washed with H2O (2×) and brine and dried over Na2SO4. After filtration, the filtrate was concentrated and the resulting residue was purified by chromatography with 9.5:0.5 hexane/EtOAc to provide desired product (14p).

Aufarbeitung

  1. customThe two layers were separated
  2. extractionthe aqueous layer was extracted with DCM (2×)
  3. washThe combined organics were washed with H2O (2×) and brine
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated
  7. customthe resulting residue was purified by chromatography with 9.5:0.5 hexane/EtOAc

Quellen und Nachweise

ORD-Eintrag
ord-a024798dfc2a43fd9f609bd0e287f79c
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08017641B2

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