Hydrazine hydrate (1:1) → HCID 178434196, compound

HRID 2084290Notes

Reaction equation

HRID 2084290 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]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 5194481,3-Cyclohexanedione, 2-acetyl-5,5-dimethyl-

Product 1

HCID 178434196HCID 178434196, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

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

  1. customprepared
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in dichloromethane
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated

Sources & evidence

ORD record
ord-7341d36ebd6943d69784ba4eecbad69a
Source dataset
uspto-grants-2004_04
Patent number
US06716856B1

Reaction notes

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