1,4-Dioxane → HCID 21455987, compound

HRID 435597Notes

Reaction equation

HRID 435597 reaction equation
[N+:1]([C:4]1[N:8]([CH3:9])[C:7]([C:10]2[N:14]3[N:15]=[C:16](Cl)[CH:17]=[CH:18][C:13]3=[N:12][N:11]=2)=[N:6][CH:5]=1)([O-:3])=[O:2].[O:20]1CCOC[CH2:21]1.C[O-].[Na+]>CO>[N+:1]([C:4]1[N:8]([CH3:9])[C:7]([C:10]2[N:14]3[N:15]=[C:16]([O:20][CH3:21])[CH:17]=[CH:18][C:13]3=[N:12][N:11]=2)=[N:6][CH:5]=1)([O-:3])=[O:2]

Participants

5

Reactant 3

HCID 312751,4-DioxaneHCID 10942334Sodium MethoxideHCID 21455925HCID 21455925, compound

Product 1

HCID 21455987HCID 21455987, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1.96 g. crude 3-(5-nitro-1-methyl-2-imidazolyl)-6- -chloro-s-triazolo[4,3-b]pyridazine was dissolved in 35 ml. of a mixture of dioxan and methanol (1:1), 0.84 g. sodium methylate added thereto, the reaction mixture heated under reflux for 1 hour, the solution then evaporated in a vacuum, the residue triturated with water, filtered with suction and dried at 120° C. in a vacuum. There was thus obtained 0.64 g. of the desired 3-(5-nitro-1-methyl-2-imidazolyl)-6-methoxy-s-triazolo[4,3-b] pyridazine, which has a melting point of 193° - 198° C.

Workup

  1. temperaturethe reaction mixture heated
  2. temperatureunder reflux for 1 hour
  3. customthe solution then evaporated in a vacuum
  4. customthe residue triturated with water
  5. filtrationfiltered with suction
  6. customdried at 120° C. in a vacuum

Sources & evidence

ORD record
ord-730311652853433c974d7a1063ce58c3
Source dataset
uspto-grants-1977_02
Patent number
US04006141

Reaction notes

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