Hydrogen Peroxide → HCID 20301446, compound

HRID 1732815Notes

Reaction equation

HRID 1732815 reaction equation
[CH3:1][N:2]([CH3:17])[C:3]([N:5]([CH3:16])[C:6]1[S:7][C:8]([S:11][CH2:12][CH2:13][CH2:14][CH3:15])=[N:9][N:10]=1)=[O:4].[OH:18]O>C(O)(=O)C>[CH3:1][N:2]([CH3:17])[C:3]([N:5]([CH3:16])[C:6]1[S:7][C:8]([S:11]([CH2:12][CH2:13][CH2:14][CH3:15])=[O:18])=[N:9][N:10]=1)=[O:4]

Participants

4

Reactant 2

HCID 784Hydrogen PeroxideHCID 54497622HCID 54497622, compound

Product 1

HCID 20301446HCID 20301446, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To a solution of 300 g of 1,1,3-trimethyl-3-(5-butylthio-1,3,4-thiadiazol-2-yl) urea in 1.9 ltr glacial acetic acid there are added in drops at room temperature and with agitation 136 g of perhydrol. The temperature then rises to 28° C. After standing for 5 days, the perhydrol excess is destroyed with manganese dioxide, the glacial acetic acid is vacuum-distilled to a very large extent, and the residue taken up in methylene chloride, is treated twice with active carbon, the solvent distilled, and the remaining oil dried in high vacuum.

Workup

  1. customthen rises to 28° C
  2. customthe perhydrol excess is destroyed with manganese dioxide
  3. distillationthe glacial acetic acid is vacuum-distilled to a very large extent
  4. additionis treated twice with active carbon
  5. distillationthe solvent distilled
  6. customthe remaining oil dried in high vacuum

Sources & evidence

ORD record
ord-f5747b0094184dc3bc5179dfbf2e3b8b
Source dataset
uspto-grants-1980_12
Patent number
US04239524

Reaction notes

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