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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
ノート
印刷プレビュー

反応式

HRID 628528 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-7707dc037b63455eb7b0a058c33de0f0
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09314023B2

反応ノート

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