Potassium Carbonate → HCID 86750964, Verbindung

HRID 1683807Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1683807
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:12][C:11](=[O:13])[NH:10][N:9]=2)=[CH:4][CH:3]=1.Cl[CH2:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH2:12][C:11](=[O:13])[N:10]([CH2:15][C:16](=[O:21])[C:17]([CH3:20])([CH3:19])[CH3:18])[N:9]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 835721-ChloropinacoloneHCID 47787935-(4-Chloro-phenyl)-2,4-dihydro-pyrazol-3-one

Produkt 1

HCID 86750964HCID 86750964, VerbindungAusbeute 104,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 3.5 g (16 mmol) of 3-(4-chlorophenyl)-4, 5-dihydropyrazol-5-one, 2.9 g (24 mmol) of chloropinacolone, 5.4 g (39 mmol) of anhydrous potassium carbonate and acetonitrile was heated under reflux for 14 hours. Excess potassium carbonate and the formed salts were removed by filtration. The filtrate was concentrated and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1 (v/v)) to give 4.9 g of the object compound as white crystals (yield 97%).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 14 hours
  3. customExcess potassium carbonate and the formed salts were removed by filtration
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1 (v/v))

Quellen und Nachweise

ORD-Eintrag
ord-ebf881da69db4ec6a2346067fc959a9b
Quelldatensatz
uspto-grants-1997_06
Patentnummer
US05639776

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