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 83494노트

반응식

HRID 83494 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

HCID 712877381-(4-Fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-1H-pyrazol-3-ylamine수율 50.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1451ea0a4c834f8fbf057590cca2cec7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846746B2

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