2-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione → HCID 68704522, Verbindung

HRID 14460Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 14460
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:20](=[O:24])[CH:21]([CH3:23])[CH3:22])[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[C:13]([F:18])[C:12]=2O)=[O:10])=[CH:4][CH:3]=1>C(O)(=O)C.Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9](=[O:10])[C:11]3[C:12](=[C:13]([F:18])[C:14]([F:17])=[CH:15][CH:16]=3)[O:24][C:20]=2[CH:21]([CH3:23])[CH3:22])=[CH:6][CH:7]=1

Komponenten

4

Edukt 1

HCID 686997002-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione

Produkt 1

HCID 68704522HCID 68704522, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 2-(4-chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione (3.65 g, 10.3 mmol) in acetic acid (36 ml) and concentrated HCl solution (2 ml) is stirred at 140° C. for 3 h. The reaction mixture is cooled to room temperature, poured onto ice-water and extracted with methylene chloride. The organic layer is washed with saturated sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo to afford the title compound as a brown solid.

Aufarbeitung

  1. temperatureThe reaction mixture is cooled to room temperature
  2. additionpoured onto ice-water
  3. extractionextracted with methylene chloride
  4. washThe organic layer is washed with saturated sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-fa224b4cc0cd49ce92d0db54d17f8641
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07732435B2

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