Hydrazine hydrate (1:1) → HCID 22288370, compound

HRID 427332Notes

Reaction equation

HRID 427332 reaction equation
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](Cl)=[N:4][N:3]=1.O.[NH2:14][NH2:15]>C(O)C>[ClH:1].[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([NH:14][NH2:15])=[N:4][N:3]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 784901,4-Dichlorophthalazine

Product 1

HCID 22288370HCID 22288370, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1,4-Dichlorophthalazine (20.0 g, 0.100 mol) was added to a boiling solution of hydrazine monohydrate (37.3 ml, 0.765 mol) in ethanol (500 ml) and the mixture heated at reflux for 0.5 h. The mixture was cooled to room temperature and the solid collected by filtration. The material was washed with ether, azeotroped with ethanol and dried in vacuo to afford the title-compound. 1H NMR (250 MHz, d6-DMSO) δ 7.72-8.35 (4H, m, 4 of Ar—H).

Workup

  1. temperaturethe mixture heated
  2. temperatureat reflux for 0.5 h
  3. filtrationthe solid collected by filtration
  4. washThe material was washed with ether
  5. customazeotroped with ethanol
  6. customdried in vacuo
  7. customto afford the title-compound

Sources & evidence

ORD record
ord-29ff49fc865943db9649fa6387014393
Source dataset
uspto-grants-2001_11
Patent number
US06313125B1

Reaction notes

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