Formic Acid → 4-(3,4,5-Trifluorophenyl)cyclohexan-1-one

HRID 1769574Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1769574
C(O)=O.C1(C)C=CC=CC=1.C1CO[C:13]2([CH2:18][CH2:17][CH:16]([C:19]3[CH:24]=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[CH:20]=3)[CH2:15][CH2:14]2)[O:12]1>O>[F:25][C:23]1[CH:24]=[C:19]([CH:16]2[CH2:15][CH2:14][C:13](=[O:12])[CH2:18][CH2:17]2)[CH:20]=[C:21]([F:27])[C:22]=1[F:26]

Komponenten

5

Edukt 3

HCID 284Formic AcidHCID 1140TolueneHCID 867484001,1-Ethylenedioxy4-(3',4',5'-trifluorophenyl)-cyclohexane

Produkt 1

HCID 219932844-(3,4,5-Trifluorophenyl)cyclohexan-1-oneAusbeute 79,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Formic acid (82.7 g) and toluene (20 ml) were added to 1,1-ethylenedioxy-4-(3',4', 5'-trifluorophenyl)cyclohexane (95.02 g), followed by heating the mixture under reflux with stirring for 2 hours, adding the reaction solution to water (500 ml), extracting with ethyl acetate (1 l), drying the organic layer over anhydrous magnesium sulfate, distilling off the solvent under reduced pressure, and recrystallizing from ethanol, to obtain 4-(3',4',5'-trifluorophenyl)cyclohexanone (63.1 g). m.p. 123.5° C.

Aufarbeitung

  1. temperatureby heating the mixture
  2. temperatureunder reflux
  3. extractionextracting with ethyl acetate (1 l)
  4. dry with materialdrying the organic layer over anhydrous magnesium sulfate
  5. distillationdistilling off the solvent under reduced pressure
  6. customrecrystallizing from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-bf938f53a585426caee9bf0f3e47c307
Quelldatensatz
uspto-grants-1995_01
Patentnummer
US05382379

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