Methylhydrazine → 1-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-one

HRID 129483ノート

反応式

HRID 129483 の反応式
[CH3:1][NH:2][NH2:3].CN([CH:7]=[C:8]1[C:13](=[O:14])[CH2:12][CH2:11][CH2:10][C:9]1=O)C>CO>[CH3:1][N:2]1[C:9]2[CH2:10][CH2:11][CH2:12][C:13](=[O:14])[C:8]=2[CH:7]=[N:3]1

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 3593532-[(Dimethylamino)methylidene]cyclohexane-1,3-dione

生成物 1

HCID 27657961-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-one収率 89.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 46.1 g (1.0 mol) of methylhydrazine in 400 ml of methanol is slowly added dropwise at ambient temperature to a solution of 167.2 g (1.0 mol) of 2-(dimethylaminomethylene)-cyclohexane-1,3-dione in 2000 ml of methanol. The reaction mixture is then refluxed for 1.5 hours. It is evaporated dryness in vacuo and the crude product obtained is purified by chromatography on silica gel (made by Baker, 30-60 μm) with a mixture of ethyl acetate and cyclohexane=9:1.

後処理

  1. temperatureThe reaction mixture is then refluxed for 1.5 hours
  2. customIt is evaporated dryness in vacuo

出典と根拠

ORDレコード
ord-f8c27671b78c49e7a431f3776f2924a6
出典データセット
uspto-grants-1995_11
特許番号
US05468766

反応ノート

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