Acetohydrazide → HCID 12726827, compound

HRID 1763598Notes

Reaction equation

HRID 1763598 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=2)=[CH:6][CH:7]=1.[C:15]([NH:18][NH2:19])(=O)[CH3:16]>C(O)CCC>[Cl:14][C:10]1[CH:9]=[C:8]([C:5]2[CH:6]=[CH:7][C:2]3[N:3]([C:15]([CH3:16])=[N:18][N:19]=3)[N:4]=2)[CH:13]=[CH:12][CH:11]=1

Participants

4

Reactant 2

HCID 14039AcetohydrazideHCID 127268113-Chloro-6-(3-chlorophenyl)pyridazine

Product 1

HCID 12726827HCID 12726827, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A mixture of 2.0 g. of 3-chloro-6-(m-chlorophenyl)pyridazine, 50 ml. of n-butanol and 1.32 g. of acetylhydrazine is refluxed for 18 hrs. The mixture is concentrated to dryness under vacuum and the residue dissolved in methylene chloride. The solution is passed through a short column of hydrous magnesium silicate. The eluent is refluxed while hexane is gradually added until crystals separated. Cooling and filtering gives 1.50 g. of crystals, m.p. 171°-172.5° C.

Workup

  1. additionA mixture of 2.0 g
  2. concentrationThe mixture is concentrated to dryness under vacuum
  3. dissolutionthe residue dissolved in methylene chloride
  4. temperatureThe eluent is refluxed while hexane
  5. additionis gradually added until crystals
  6. customseparated
  7. temperatureCooling
  8. filtrationfiltering
  9. customgives 1.50 g

Sources & evidence

ORD record
ord-90a0382e726845c4b3b669e9f3f9010d
Source dataset
uspto-grants-1978_09
Patent number
US04112095

Reaction notes

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