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

HRID 129483Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 129483
[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

Komponenten

4

Edukt 2

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

Produkt 1

HCID 27657961-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-oneAusbeute 89,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-f8c27671b78c49e7a431f3776f2924a6
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05468766

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