Acetic Acid → HCID 23452463, compound

HRID 1278331Notes

Reaction equation

HRID 1278331 reaction equation
[CH:1]1([CH2:7][NH:8][C:9]([C:11]2[S:12][C:13](SC)=[N:14][N:15]=2)=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Mn]([O-])(=O)(=O)=O.[K+].[S:24](S([O-])=O)([O-:27])(=O)=[O:25].[Na+].[Na+].[C:33](O)(=O)C>O.[O-2].[O-2].[Mn+4]>[CH:1]1([CH2:7][NH:8][C:9]([C:11]2[S:12][C:13]([S:24]([CH3:33])(=[O:27])=[O:25])=[N:14][N:15]=2)=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

7

Reactant 4

HCID 176Acetic AcidHCID 516875Potassium PermanganateHCID 656671Sodium PyrosulfiteHCID 54531929HCID 54531929, compound

Product 1

HCID 23452463HCID 23452463, compound

Reagents, catalysts & solvents 2

HCID 178418406HCID 178418406, compoundCatalystHCID 962WaterSolvent2×

Conditions

Temperature
70 °C

Procedure

20.3 g of 5-methylthio-1,3,4-thiadiazole-2-carboxylic acid cyclohexylmethylamide were dissolved in 130 ml acetic acid and 25 ml water. 16 g pulverized potassium permanganate was then introduced upon stirring to cause the temperature to increase to 70° C. Thereafter, stirring was continued for 30 minutes. The mixture was cooled and then mixed with 300 ml ice water. The formed manganese dioxide was reduced with a solution of 14.3 g sodium metabisulfite in 100 ml water. The precipitated compound was removed by suction and recrystallized from ethanol.

Workup

  1. additionwas then introduced
  2. stirringThereafter, stirring
  3. temperatureThe mixture was cooled
  4. customThe precipitated compound was removed by suction
  5. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-910245bd2164460db4f8c359110f9c79
Source dataset
uspto-grants-1981_07
Patent number
US04281121

Reaction notes

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