1-(4-Fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-4,5-dihydro-1H-pyrazol-3-ylamine → 1-(4-Fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-1H-pyrazol-3-ylamine

HRID 83494Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 83494
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:23])([F:22])[F:21])[CH:14]=3)[CH2:11][C:10]([NH2:24])=[N:9]2)=[CH:4][CH:3]=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][C:20]([F:21])([F:23])[F:22])[CH:14]=3)=[CH:11][C:10]([NH2:24])=[N:9]2)=[CH:4][CH:3]=1

Komponenten

3

Edukt 1

HCID 712877431-(4-Fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-4,5-dihydro-1H-pyrazol-3-ylamine

Produkt 1

HCID 712877381-(4-Fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-1H-pyrazol-3-ylamineAusbeute 50,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a solution of 1-(4-fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-4,5-dihydro-1H-pyrazol-3-ylamine (1.29 g) in toluene (10 ml) was added activated carbon (pH5 to 8, 0.64 g), and the mixture was stirred for 2 hours under oxygen atmosphere under cooling to reflux. After cooling to room temperature, the activated carbon was filtered off through Celite eluting with ethyl acetate. This filtrate was concentrated under reduced pressure. To the resulting residue, a mixed solvent of diisopropyl ether/n-hexane was added and the mixture was stirred at room temperature. The insoluble substance was collected by filtration, and then dried under reduced pressure to give the titled compound (652 mg).

Aufarbeitung

  1. temperatureunder cooling
  2. temperatureto reflux
  3. filtrationthe activated carbon was filtered off through Celite
  4. washeluting with ethyl acetate
  5. concentrationThis filtrate was concentrated under reduced pressure
  6. additionTo the resulting residue, a mixed solvent of diisopropyl ether/n-hexane was added
  7. stirringthe mixture was stirred at room temperature
  8. filtrationThe insoluble substance was collected by filtration
  9. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1451ea0a4c834f8fbf057590cca2cec7
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846746B2

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