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4,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine → 1-(4-Fluorophenyl)-5-[4-(methylthio)phenyl]-3-pyrazolamine

HRID 654775
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인쇄 미리보기

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HRID 654775 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:12]([C:13]3[CH:18]=[CH:17][C:16]([S:19][CH3:20])=[CH:15][CH:14]=3)[CH2:11][C:10]([NH2:21])=[N:9]2)=[CH:4][CH:3]=1>ClCCl.[O-2].[Mn+4].[O-2]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([S:19][CH3:20])=[CH:15][CH:14]=3)=[CH:11][C:10]([NH2:21])=[N:9]2)=[CH:6][CH:7]=1
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참가 물질

4

반응물 1

HCID 104945294,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine

생성물 1

HCID 107565811-(4-Fluorophenyl)-5-[4-(methylthio)phenyl]-3-pyrazolamine수율 64.4%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of 4,5-dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine (1 g) and manganese (IV) oxide (1.16 g) in dichloromethane (100 ml) was stirred at ambient temperature for 2 hours. The insoluble was filtered and the filtrate was concentrated to dryness. The residue (1 g) was purified by column chromatography on silica gel (16 g) eluting with a mixture of chloroform and ethyl acetate (5:1 to give a pale brown powder of 1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine (0.64 g).

후처리

  1. filtrationThe insoluble was filtered
  2. concentrationthe filtrate was concentrated to dryness
  3. customThe residue (1 g) was purified by column chromatography on silica gel (16 g)
  4. washeluting with a mixture of chloroform and ethyl acetate (5:1

출처 및 근거

ORD 기록
ord-c1edf38799ef42efae8da5373a03e824
출처 데이터셋
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05134142

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