Ethyl trifluoroacetate → 1-(2,5-Difluorophenyl)-4,4,4-trifluorobutane-1,3-dione

HRID 260939

Reaktionsgleichung

Reaktionsgleichung von HRID 260939
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[F:11])=[O:3].[F:12][C:13]([F:20])([F:19])[C:14](OCC)=[O:15].C[O-].[Na+]>CCOCC.CO>[F:11][C:5]1[CH:6]=[CH:7][C:8]([F:10])=[CH:9][C:4]=1[C:2](=[O:3])[CH2:1][C:14]([C:13]([F:20])([F:19])[F:12])=[O:15]

Komponenten

6

Edukt 3

HCID 9794Ethyl trifluoroacetateHCID 747941-(2,5-Difluorophenyl)ethan-1-oneHCID 10942334Sodium Methoxide

Produkt 1

HCID 152785581-(2,5-Difluorophenyl)-4,4,4-trifluorobutane-1,3-dioneAusbeute 91,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

28.5 g of 2,5-difluoroacetophenone and 26 g of ethyl trifluoroacetate were stirred in 400 ml of anhydrous ether and cooled in an ice bath. 42 ml of 25 wt % sodium methoxide in methanol was then added over 5 minutes. After stirring 1 hour at room temperature, the reaction mixture was extracted with water, the water acidified and extracted with methylene chloride to give 42 g of 1-(2,5-difluorophenyl)-3-(trifluoromethyl)-propane-1,3-dione.

Aufarbeitung

  1. temperaturecooled in an ice bath
  2. extractionthe reaction mixture was extracted with water
  3. extractionextracted with methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-14a563864e5c498c8d154d9a736fe19e
Quelldatensatz
uspto-grants-1996_06
Patentnummer
US05530126

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