Hydrogen Peroxide → HCID 21842428, compound

HRID 1737239Notes

Reaction equation

HRID 1737239 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=2[Cl:15])[N:5]=[C:4]([N:16]2[CH2:21][CH2:20][S:19][CH2:18][CH2:17]2)[N:3]=1.OO.S([O-])([O-])=[O:25].[Na+].[Na+]>C(O)(=O)C>[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=2[Cl:15])[N:5]=[C:4]([N:16]2[CH2:17][CH2:18][S:19](=[O:25])[CH2:20][CH2:21]2)[N:3]=1

Participants

5

Reactant 3

HCID 784Hydrogen Peroxide2×HCID 24437Sodium SulfiteHCID 21842440HCID 21842440, compound

Product 1

HCID 21842428HCID 21842428, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

In 150 ml of acetic acid was dissolved 2.0 g of the compound synthesized in Example 38. To this solution was added 1.3 ml of 30% aqueous solution of hydrogen peroxide dropwise under ice-cooling and the mixture was stirred at the same temperature for 3 hours. The excess of hydrogen peroxide was decomposed with aqueous sodium sulfite solution and the mixture was concentrated. The crystals separated out were collected by filtration, rinsed with water, and dried to provide 1.86 g of the title compound as white crystals. m.p. 267-269° C.

Workup

  1. temperaturecooling
  2. concentrationthe mixture was concentrated
  3. customThe crystals separated out
  4. filtrationwere collected by filtration
  5. washrinsed with water
  6. customdried

Sources & evidence

ORD record
ord-14943cff5a9f43738834df65d0d425de
Source dataset
uspto-grants-1999_10
Patent number
US05962453

Reaction notes

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