Sodium Sulfate → 4-Phenyl-1,2,4-triazoline-3,5-dione

HRID 1658681Notes

Reaction equation

HRID 1658681 reaction equation
[C:1]1([N:7]2[C:11](=[O:12])[NH:10][NH:9][C:8]2=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S([O-])([O-])(=O)=O.[Na+].[Na+].[N+]([O-])=O>C(Cl)Cl>[C:1]1([N:7]2[C:8](=[O:13])[N:9]=[N:10][C:11]2=[O:12])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

5

Reactant 3

HCID 24436Sodium SulfateHCID 852294-Phenylurazole2×HCID 178526396Nitrogen Dioxide

Product 1

HCID 779134-Phenyl-1,2,4-triazoline-3,5-dione

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

4-Phenylurazole (25gm) and anhydrous sodium sulphate were suspended in methylene chloride. The suspension was cooled in ice and nitrogen dioxide was passed in until all the 4-phenylurazole dissolved. The solution was filtered and the solvent removed under reduced pressure. The solid was either used as obtained or purified by sublimation (at 100°C and 10-5 mm of mercury).

Workup

  1. temperatureThe suspension was cooled in ice
  2. dissolutiondissolved
  3. filtrationThe solution was filtered
  4. customthe solvent removed under reduced pressure
  5. customas obtained
  6. custompurified by sublimation (at 100°C and 10-5 mm of mercury)

Sources & evidence

ORD record
ord-58368f047bbe4262b595d93c361d58b2
Source dataset
uspto-grants-1976_06
Patent number
US03966530

Reaction notes

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