1-Butanol → HCID 20310397, compound

HRID 1763599Notes

Reaction equation

HRID 1763599 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([Cl:15])[CH:10]=2)=[CH:6][C:7]=1[CH3:8].C(O)CCC.[C:21]([NH:24][NH2:25])(=O)[CH3:22].[Si]([O-])([O-])([O-])[O-].[Mg+2].[Mg+2]>C(Cl)Cl.CCCCCC>[Cl:15][C:11]1[CH:10]=[C:9]([C:5]2[CH:6]=[C:7]([CH3:8])[C:2]3[N:3]([C:21]([CH3:22])=[N:24][N:25]=3)[N:4]=2)[CH:14]=[CH:13][CH:12]=1

Participants

7

Reactant 4

HCID 2631-ButanolHCID 14039AcetohydrazideHCID 66225Magnesium orthosilicateHCID 144502203-Chloro-6-(3-chlorophenyl)-4-methylpyridazine

Product 1

HCID 20310397HCID 20310397, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 8058HexaneSolvent

Procedure

A mixture of 7.17 g. of 3-chloro-6-(m-chlorophenyl)-4-methylpyridazine, 100 ml. of n-butanol and 6.96 g. of acetylhydrazine is refluxed overnight. The mixture is coated and filtered to give solid. The solid is dissolved in methylene chloride and the solution 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 3.30 g. of crystals, m.p. 193.5°-195.5° C.

Workup

  1. additionA mixture of 7.17 g
  2. filtrationfiltered
  3. customto give solid
  4. additionis gradually added until crystals
  5. customseparated
  6. temperatureCooling
  7. filtrationfiltering
  8. customgives 3.30 g

Sources & evidence

ORD record
ord-25e26cb94a2a4ccabca3cb5350e7f396
Source dataset
uspto-grants-1978_09
Patent number
US04112095

Reaction notes

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