Phenylhydrazine → HCID 59436173、化合物

HRID 1895280ノート

反応式

HRID 1895280 の反応式
C[N:2]([CH:4]=[N:5][C:6]([C:8]1[C:13](=[O:14])[CH:12]=[CH:11][N:10]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)[N:9]=1)=O)C.[C:25]1([NH:31]N)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(O)(=O)C>[C:25]1([N:31]2[C:6]([C:8]3[C:13](=[O:14])[CH:12]=[CH:11][N:10]([C:15]4[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=4)[N:9]=3)=[N:5][CH:4]=[N:2]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

4

反応物 2

HCID 7516PhenylhydrazineHCID 59436171HCID 59436171、化合物

生成物 1

HCID 59436173HCID 59436173、化合物収率 93.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
120 °C

実験手順

A solution of N-[(dimethylamino)methylidene]-4-oxo-1-[3-(trifluoromethyl)phenyl]-1,4-dihydropyridazine-3-carboxamide (0.119 g, 0.35 mmol) in acetic acid (5.0 mL) was treated with phenyl hydrazine (0.070 mL, 0.71 mmol). The resulting solution was heated under microwave heating conditions at 120° C. for 10 min. After that time the reaction was cooled to room temperature and the crude product purified by flash column chromatography (silica gel, ethyl acetate to 85:15 ethyl acetate/methanol) to give a colorless solid that was recrystallized from ethyl acetate/hexanes to give 0.126 g (46%) of 3-(1-phenyl-1H-1,2,4-triazol-5-yl)-1-[3-(trifluoromethyl)phenyl]pyridazin-4(1H)-one as colorless crystals.

後処理

  1. temperatureThe resulting solution was heated under microwave
  2. temperatureAfter that time the reaction was cooled to room temperature
  3. customthe crude product purified by flash column chromatography (silica gel, ethyl acetate to 85:15 ethyl acetate/methanol)
  4. customto give a colorless solid
  5. customthat was recrystallized from ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-d9de4af5b6194d888f36039697d2c578
出典データセット
uspto-grants-2013_08
特許番号
US08513251B2

反応ノート

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