Hydrogen Peroxide → HCID 22394127, compound
Reaction equation
[CH2:1]([O:3][CH2:4][CH2:5][S:6][C:7]1[S:8][CH:9]=[C:10]([C:12]2[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=2)[N:11]=1)[CH3:2].OO.C(=O)([O-])[OH:21].[Na+]>C(O)(=O)C.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH2:1]([O:3][CH2:4][CH2:5][S:6]([C:7]1[S:8][CH:9]=[C:10]([C:12]2[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=2)[N:11]=1)=[O:21])[CH3:2]Participants
7
Procedure
Dissolved in 1.7 ml of acetic acid were 0.33 g (1.24 mmol) of the compound obtained in Example 1, and 0.15 ml (1.32 mmol) of a 30% aqueous solution of hydrogen peroxide and a catalytic amount of sodium tungstate were successively added to the solution, which was stirred at room temperature for 4 hours. The reaction solution was poured in 34 ml of water, neutralized with sodium hydrogencarbonate and extracted with 34 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 0.27 g of white crystalline powders (77% yield).
Workup
- extractionextracted with 34 ml of chloroform
- customAfter separation of the chloroform layer
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- customThe residues were purified by silica gel chromatography
Sources & evidence
- ORD record
- ord-5299d1424a784cd28d80e0db2dab82ed
- Source dataset
- uspto-grants-1992_12
- Patent number
- US05171746
Reaction notes
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