Hydrogen Peroxide → HCID 178496538, compound

HRID 1413660Notes

Reaction equation

HRID 1413660 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][S:5][C:6]1[N:10]=[CH:9][NH:8][N:7]=1.[OH:11]O>[Pd].C(O)(=O)C>[CH3:1][O:2][CH2:3][CH2:4][S:5]([C:6]1[N:10]=[CH:9][NH:8][N:7]=1)=[O:11]

Participants

5

Reactant 2

HCID 784Hydrogen PeroxideHCID 178496535HCID 178496535, compound

Product 1

HCID 178496538HCID 178496538, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 176Acetic AcidSolvent

Procedure

A solution of 31.8 g. of 3-(2-methoxyethylthio)-1,2,4-triazole was dissolved in 300 ml. of acetic acid and heated to 80° C. To this solution was added by portions 67.2 ml. of 100 vol. hydrogen peroxide and the temperature was maintained at 80° C. for two hours with cooling as necessary in the early stages. A small amount of 10% palladium/charcoal catalyst was added to destroy excess hydrogen peroxide. After an hour the solution was filtered and sulphur dioxide passed through the mixture as a precaution in case peroxides had been formed. The solution was vacuum evaporated and crystals of the sulphonyl compound were removed. On the addition of further petroleum ether to the liquors, filtration and vacuum distillation, there was obtained an oily liquid, 3-(2-methoxyethylsulphinyl)-1,2,4-triazole. Elemental analysis satisfactory.

Workup

  1. additionTo this solution was added by portions 67.2 ml
  2. temperaturewith cooling as necessary in the early stages
  3. customto destroy excess hydrogen peroxide
  4. filtrationAfter an hour the solution was filtered
  5. customhad been formed
  6. customevaporated
  7. customcrystals of the sulphonyl compound were removed
  8. additionOn the addition of further petroleum ether
  9. filtrationto the liquors, filtration and vacuum distillation

Sources & evidence

ORD record
ord-3ae77ec1406049e39a0f5afcb774e3d0
Source dataset
uspto-grants-1981_02
Patent number
US04251262

Reaction notes

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