Hydrogen Peroxide → HCID 9930407, compound

HRID 356693Notes

Reaction equation

HRID 356693 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][C:10]([C:19]3[CH:24]=[CH:23][C:22]([S:25]([CH3:27])=[O:26])=[CH:21][CH:20]=3)=[CH:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.[OH:28]O>CO.C(OCC)(=O)C.O.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[NH:9][C:10]([C:19]3[CH:24]=[CH:23][C:22]([S:25]([CH3:27])(=[O:28])=[O:26])=[CH:21][CH:20]=3)=[CH:11][C:12]=2[C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[CH:6][CH:7]=1

Participants

6

Reactant 2

HCID 784Hydrogen Peroxide2×HCID 9885993188352-45-6

Product 1

HCID 9930407HCID 9930407, compound

Reagents, catalysts & solvents 3

HCID 150191Sodium Tungstate DihydrateCatalystHCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

0.5 g (1.4 mmol) of the product of Example 44 was dissolved in a mixture of 4 mL of methanol and 16 mL of ethyl acetate. The solution was treated 0.045 g sodium tungstate dihydrate and 0.63 mL (5.6 mmol) of 30% hydrogen peroxide solution while heating at reflux over a period of 4 hours. A further 0.3 mL (2.8 mmol) hydrogen peroxide was added. The mixture was refluxed overnight and then cooled to room temperature. A white solid was recovered by filtration and was washed with water to provide the desired product.

Workup

  1. temperaturewhile heating
  2. temperatureat reflux over a period of 4 hours
  3. temperatureThe mixture was refluxed overnight
  4. filtrationA white solid was recovered by filtration
  5. washwas washed with water

Sources & evidence

ORD record
ord-2b9e0c94d07b44cab7bd1db3662517a9
Source dataset
uspto-grants-1998_11
Patent number
US05837719

Reaction notes

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