Hydrogen Peroxide → HCID 12889533, compound

HRID 1164316Notes

Reaction equation

HRID 1164316 reaction equation
[CH2:1]([S:3][C:4]1[S:5][C:6]([S:9]([CH2:12][CH2:13][CH2:14][CH3:15])(=[O:11])=[O:10])=[N:7][N:8]=1)[CH3:2].[OH:16]O.O>C(O)(=O)C>[CH2:1]([S:3]([C:4]1[S:5][C:6]([S:9]([CH2:12][CH2:13][CH2:14][CH3:15])(=[O:11])=[O:10])=[N:7][N:8]=1)=[O:16])[CH3:2]

Participants

5

Procedure

A solution of 53.29 g of 2-Ethylthio-5-butylsulfonyl-1,3,4-thiadiazole in 500 ml acetic acid is mixed with 23 g of 30 percent hydrogen peroxide. The reaction takes place over night upon standing at room temperature. Then one liter water is added to the reaction solution, the separated oil is extracted with dichloromethane, the extract is freed from acetic acid by extraction with soda ash solution, the dichloromethane phase is dried with magnesium sulfate and the solvent is distilled off completely, finally in vacuo. The remaining residue is recrystallized from isopropylether/isopropanol.

Workup

  1. customupon standing at room temperature
  2. extractionthe separated oil is extracted with dichloromethane
  3. extractionthe extract is freed from acetic acid by extraction with soda ash solution
  4. dry with materialthe dichloromethane phase is dried with magnesium sulfate
  5. distillationthe solvent is distilled off completely
  6. customThe remaining residue is recrystallized from isopropylether/isopropanol

Sources & evidence

ORD record
ord-df315cee3b8a4c598f252b92f88f58d0
Source dataset
uspto-grants-1983_01
Patent number
US04369185

Reaction notes

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