Pyrazole → 1-Phenyl-2-(1H-pyrazol-1-yl)ethanone

HRID 133474

Reaktionsgleichung

Reaktionsgleichung von HRID 133474
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[NH:11]1[CH:15]=[CH:14][CH:13]=[N:12]1.C([O-])([O-])=O.[K+].[K+]>CC#N.CCOC(C)=O>[C:5]1([C:3](=[O:4])[CH2:2][N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

6

Edukt 3

HCID 1048PyrazoleHCID 107572-ChloroacetophenoneHCID 11430Potassium Carbonate

Produkt 1

HCID 27663751-Phenyl-2-(1H-pyrazol-1-yl)ethanone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 1.5 g (9.7 mmol) of 2-chloroacetophenone in 10 mL of MeCN, 0.7 g (10.3 mmol) of pyrazole was added. After all the solids dissolved, 1.4 g (10.1 mmol) of ground K2CO3 was added and the mixture was stirred for 5 h. The reaction was diluted with EtOAc, filtered, and the solid was washed with EtOAc. The filtrate was washed with water and brine, then was dried and concentrated. The residue was chromatographed on a flash column using a gradient of 10-50% EtOAc-hexane to isolate desired product.

Aufarbeitung

  1. dissolutionAfter all the solids dissolved
  2. filtrationfiltered
  3. washthe solid was washed with EtOAc
  4. washThe filtrate was washed with water and brine
  5. customwas dried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on a flash column

Quellen und Nachweise

ORD-Eintrag
ord-1eabe1ca28e24df185018b6299bd77d2
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07390835B2

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