Piperazine → HCID 5298668, compound

HRID 1608659Notes

Reaction equation

HRID 1608659 reaction equation
[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1Cl.[NH:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1>C(O)C>[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 1204623(2H)-Pyridazinone, 4,5-dichloro-2-methyl-

Product 1

HCID 5298668HCID 5298668, compoundYield 60.2%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 4.48 g (25 mmoles) of 4,5-dichloro-2-methyl-3(2H)-pyridazinone and 17.2 g (200 mmoles) of piperazine in 45 ml of anhydrous ethanol is boiled for 4 hours under stirring and reflux cooling. The solvent is evaporated in vacuo and the residue is dissolved in a mixture of water and dichloromethane. The organic phase is washed with water, dried and evaporated. The residue is triturated with ether. Thus 3.44 g (60%) of the desired compound are obtained. M.p.: 83°-87° C.

Workup

  1. temperaturereflux
  2. temperaturecooling
  3. customThe solvent is evaporated in vacuo
  4. dissolutionthe residue is dissolved in a mixture of water and dichloromethane
  5. washThe organic phase is washed with water
  6. customdried
  7. customevaporated
  8. customThe residue is triturated with ether

Sources & evidence

ORD record
ord-a7b4e4cd5e9a4ffebf5ce22faeb0de6b
Source dataset
uspto-grants-1995_03
Patent number
US05395934

Reaction notes

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