Hydrogen Peroxide → HCID 11459567, compound

HRID 2113474Notes

Reaction equation

HRID 2113474 reaction equation
ClCCl.[N+:4]([C:7]1[CH:16]=[C:15]2[C:10]([CH2:11][O:12][C:13]2=[O:14])=[CH:9][CH:8]=1)([O-:6])=[O:5].[Br:17]Br.OO>O>[N+:4]([C:7]1[CH:16]=[C:15]2[C:10]([CH:11]([Br:17])[O:12][C:13]2=[O:14])=[CH:9][CH:8]=1)([O-:6])=[O:5]

Participants

6

Reactant 4

HCID 784Hydrogen Peroxide2×HCID 6344DichloromethaneHCID 24408BromineHCID 2235846-Nitrophthalide

Product 1

HCID 11459567HCID 11459567, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 125 ml of a dichloromethane solution of 6-nitrophtalide (8.0 g, 0.047 mol), bromine (8.25 g, 0.052 mol, 1.15 eq) and hydrogen peroxide (5.07 g of a 35% solution in water, equivalent to 1.77 of hydrogen peroxide, 0.052 mol, 1.15 eq) were added. The mixture was gently refluxed for 11 hours, then cooled down and concentrated by solvent evaporation. The aqueous layer was separated, and the organic phase washed with water before drying up (Na2SO4).

Workup

  1. temperatureThe mixture was gently refluxed for 11 hours
  2. temperaturecooled down
  3. concentrationconcentrated by solvent evaporation
  4. customThe aqueous layer was separated
  5. washthe organic phase washed with water
  6. dry with materialbefore drying up (Na2SO4)

Sources & evidence

ORD record
ord-93d7c6d3622d4000a60d11f541c99263
Source dataset
uspto-grants-2008_10
Patent number
US07432263B2

Reaction notes

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