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Methylhydrazine → 5-(4-methoxy-2,5-dimethyl-phenyl)-2-methyl-3-trifluoromethyl-3,4-dihydro-2H-pyrazole-3-ol

HRID 628528
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HRID 628528 반응식
[F:1][C:2]([F:19])([F:18])[C:3](=[O:17])[CH2:4][C:5]([C:7]1[CH:12]=[C:11]([CH3:13])[C:10]([O:14][CH3:15])=[CH:9][C:8]=1[CH3:16])=O.[CH3:20][NH:21][NH2:22]>C(O)C>[CH3:15][O:14][C:10]1[C:11]([CH3:13])=[CH:12][C:7]([C:5]2[CH2:4][C:3]([C:2]([F:19])([F:18])[F:1])([OH:17])[N:21]([CH3:20])[N:22]=2)=[C:8]([CH3:16])[CH:9]=1.[CH3:15][O:14][C:10]1[C:11]([CH3:13])=[CH:12][C:7]([C:5]2[N:21]([CH3:20])[N:22]=[C:3]([C:2]([F:19])([F:18])[F:1])[CH:4]=2)=[C:8]([CH3:16])[CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6061MethylhydrazineHCID 985795504,4,4-Trifluoro-1-(4-methoxy-2,5-dimethyl-phenyl)-butane-1,3-dione

생성물 2

HCID 1182363955-(4-methoxy-2,5-dimethyl-phenyl)-2-methyl-3-trifluoromethyl-3,4-dihydro-2H-pyrazole-3-olHCID 1182364825-(4-methoxy-2,5-dimethyl-phenyl)-1-methyl-3-trifluoromethyl-1H-pyrazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

At 0° C., to a mixture of 4,4,4-trifluoro-1-(4-methoxy-2,5-dimethyl-phenyl)-butane-1,3-dione (described in Reference Preparation example 83) 6.8 g and ethanol 100 ml was added methyl hydrazine 1.7 g. The resulting mixture was raised to room temperature and was stirred for one hour. The reaction mixture was concentrated under reduced pressure and the resulting residue was subjected to a silica gel column chromatography to give 5-(4-methoxy-2,5-dimethyl-phenyl)-2-methyl-3-trifluoromethyl-3,4-dihydro-2H-pyrazole-3-ol 3.2 g and 5-(4-methoxy-2,5-dimethyl-phenyl)-1-methyl-3-trifluoromethyl-1H-pyrazole 3 g.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7707dc037b63455eb7b0a058c33de0f0
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09314023B2

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