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 83494ノート

反応式

HRID 83494 の反応式
[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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1451ea0a4c834f8fbf057590cca2cec7
出典データセット
uspto-grants-2014_09
特許番号
US08846746B2

反応ノート

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