Hydrochloric Acid → 1,1,1-Trifluoro-2-hexanone

HRID 893534Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 893534
[Mg].[CH2:2](Br)[CH2:3][CH2:4][CH3:5].[F:7][C:8]([F:13])([F:12])[C:9](O)=[O:10].Cl>CCOCC>[F:7][C:8]([F:13])([F:12])[C:9](=[O:10])[CH2:2][CH2:3][CH2:4][CH3:5]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 8002Butyl bromideHCID 5462224Magnesium

Produkt 1

HCID 2382921,1,1-Trifluoro-2-hexanoneAusbeute 51,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel3×

Versuchsvorschrift

In a nitrogen atmosphere, 9.12 g (380 mM) of magnesium into 120 ml of ether, and 49.32 g (360 mM) of butyl bromide dissolved in 30 ml of ether was added thereto, followed by 1.5 hours of heat refluxing. After cooling by standing and with ice, 13.68 g (120 mM) of trifluoroacetic acid dissolved in 30 ml of ether was added. After being stirred for 7 hours under cooling with ice, the system was subjected to hydrolysis with addition of hydrochloric acid, followed by extraction with ether and drying of the resultant ether layer with anhydrous sodium sulfate. The dried product was distilled under normal pressure to obtain 9.46 g of 1,1,1-trifluoro-2-hexanone. Yield: 47%.

Aufarbeitung

  1. additionwas added
  2. temperatureof heat
  3. temperaturerefluxing
  4. temperatureAfter cooling
  5. additionwas added
  6. temperatureunder cooling with ice
  7. extractionfollowed by extraction with ether
  8. dry with materialdrying of the resultant ether layer with anhydrous sodium sulfate
  9. distillationThe dried product was distilled under normal pressure

Quellen und Nachweise

ORD-Eintrag
ord-e1c7157d4e1c45028c7d5f21ea1dc8af
Quelldatensatz
uspto-grants-1992_06
Patentnummer
US05126071

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