Hydrazine → HCID 178434370, compound

HRID 1291227Notes

Reaction equation

HRID 1291227 reaction equation
[C:1]([C:4]1[C:5](=[O:17])[N:6]([C:13]([CH3:16])([CH3:15])[CH3:14])[N:7]=[CH:8][C:9]=1[N:10](C)C)(=O)[CH3:2].[NH2:18]N>C(O)C>[C:13]([N:6]1[C:5](=[O:17])[C:4]2[C:1]([CH3:2])=[N:18][NH:10][C:9]=2[CH:8]=[N:7]1)([CH3:16])([CH3:15])[CH3:14]

Participants

4

Reactant 2

HCID 9321HydrazineHCID 18919343HCID 18919343, compound

Product 1

HCID 178434370HCID 178434370, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

4-Acetyl-2-t-butyl-5-dimethylamino-3(2H)-pyridazinone (2.5 g) was added to hydrazine (3.2 g)/ethanol (30 ml) and the mixture was refluxed for 6 hours. After the ethanol-hydrazine was distilled off, the residue was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was washed with n-hexane and diethyl ether and dried. White powder, 1.7 g. 1H-NMR (CDCl3) 6: 1.70(9H,s), 2.74(3H,s), 8.10(1H,s).

Workup

  1. temperaturethe mixture was refluxed for 6 hours
  2. distillationAfter the ethanol-hydrazine was distilled off
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated aqueous NaCl solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated to dryness
  7. washThe residue was washed with n-hexane and diethyl ether
  8. customdried

Sources & evidence

ORD record
ord-c6d1d4a82ee747c0877f2a8b337b04d3
Source dataset
uspto-grants-1998_05
Patent number
US05753664

Reaction notes

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