Reaction equation
[C:1]([CH:4]1[C:9](=[O:10])[CH2:8][C:7]([CH3:12])([CH3:11])[CH2:6][C:5]1=O)(=O)[CH3:2].O.[NH2:15][NH2:16]>C(O)C>[CH3:2][C:1]1[C:4]2[C:9](=[O:10])[CH2:8][C:7]([CH3:12])([CH3:11])[CH2:6][C:5]=2[NH:16][N:15]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 2-acetyl-5,5-dimethyl-cyclohexane-1,3-dione (2 g, 11.04 mmol), prepared as described in example 2, and hydrazine hydrate (1.66 ml, 33.13 mmol) in ethanol (25 ml) was stirred at room temperature for about 3 hours and then the solvent was evaporated. The residue was dissolved in dichloromethane, washed with water and brine, dried over sodium sulfate and evaporated. The title compound was obtained after chromatography on silica gel (dichloromethane:methanol=95:5) as a colourless solid (0.8 g, 45%): m.p. 103-104° C.
Workup
- customprepared
- customthe solvent was evaporated
- dissolutionThe residue was dissolved in dichloromethane
- washwashed with water and brine
- dry with materialdried over sodium sulfate
- customevaporated
Sources & evidence
- ORD record
- ord-7341d36ebd6943d69784ba4eecbad69a
- Source dataset
- uspto-grants-2004_04
- Patent number
- US06716856B1
Linked notes
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