Hydrogen Peroxide → HCID 9883994, compound

HRID 1681337Notes

Reaction equation

HRID 1681337 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([S:10][CH2:11][CH2:12][N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)=[N:7][C:6]=2[CH:19]=1.OO.C(=O)([O-])[OH:23].[Na+]>C(O)(=O)C.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([S:10]([CH2:11][CH2:12][N:13]3[CH2:14][CH2:15][O:16][CH2:17][CH2:18]3)=[O:23])=[N:7][C:6]=2[CH:19]=1

Participants

7

Reactant 3

HCID 784Hydrogen PeroxideHCID 516892Sodium BicarbonateHCID 19806312HCID 19806312, compound

Product 1

HCID 9883994HCID 9883994, compound

Reagents, catalysts & solvents 3

HCID 26052Sodium tungstateCatalystHCID 176Acetic AcidSolventHCID 962WaterSolvent

Procedure

Dissolved in 4 ml of acetic acid were 0.80 g (2.5 mmol) of the compound obtained in Example 31, and 0.37 ml (3.3 mmol) of a 30% aqueous solution of hydrogen peroxide and a catalytic quantity of sodium tungstate were successively added to the solution, which was stirred at room temperature for 1 hour. The solution was poured in 80 ml of water, neutralized with sodium hydrogencarbonate and extracted with 80 ml of chloroform. After separation of the chloroform layer, the organic layer was dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residues were purified by silica gel chromatography to obtain 0.52 g of the title compound in the form of white crystalline powders (62% yield).

Workup

  1. extractionextracted with 80 ml of chloroform
  2. customAfter separation of the chloroform layer
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residues were purified by silica gel chromatography

Sources & evidence

ORD record
ord-300ccbbb2e97445cae53f79ef0927387
Source dataset
uspto-grants-1992_12
Patent number
US05171746

Reaction notes

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