Acetic Acid → 4'-Fluoro-2-(4-trifluoromethylphenyl)acetophenone

HRID 968076

Reaktionsgleichung

Reaktionsgleichung von HRID 968076
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](N(C)C)=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C(O)(=[O:25])C.Cl>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:25])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 697465101-(4-fluorophenyl)-2-(4-trifluoromethylphenyl)-N,N-dimethylethenylamine

Produkt 1

HCID 98172164'-Fluoro-2-(4-trifluoromethylphenyl)acetophenoneAusbeute 90,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Into a 200 ml four-necked flask equipped with a thermometer, a stirrer and a reflux condenser, 15.5 g (50 mmol) of 1-(4-fluorophenyl)-2-(4-trifluoromethylphenyl)-N,N-dimethylethenylamine, 80 ml of acetic acid and 30 ml of concentrated hydrochloric acid were charged and reacted with stirring for two hours under refluxing under heating by an oil bath. After completion of reaction, 500 ml of water was added, and precipitated crystals were collected by filtration and washed with a 2% sodium hydrogen carbonate aqueous solution and water. Then, the crystals were further washed and purified with 20 ml of n-hexane and then vacuum-dried to obtain 12.7 g (yield: 90.3%) of the desired compound (melting point: 93-95° C.) as slightly yellow crystals.

Aufarbeitung

  1. additionwere charged
  2. customreacted
  3. temperatureunder refluxing
  4. temperatureunder heating by an oil bath
  5. additionwas added
  6. customprecipitated crystals
  7. filtrationwere collected by filtration
  8. washwashed with a 2% sodium hydrogen carbonate aqueous solution and water
  9. washThen, the crystals were further washed
  10. custompurified with 20 ml of n-hexane
  11. customvacuum-dried

Quellen und Nachweise

ORD-Eintrag
ord-d32059cc5c3346b889444bdb232ea8aa
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06956132B2

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