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

HRID 129483

반응식

HRID 129483 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f8c27671b78c49e7a431f3776f2924a6
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468766

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