Methylhydrazine → 1-Methyl-1,5,6,7-tetrahydro-4H-indazol-4-one
Reaction equation
[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]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
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.
Workup
- temperatureThe reaction mixture is then refluxed for 1.5 hours
- customIt is evaporated dryness in vacuo
Sources & evidence
- ORD record
- ord-f8c27671b78c49e7a431f3776f2924a6
- Source dataset
- uspto-grants-1995_11
- Patent number
- US05468766
Reaction notes
Loading…