Hydrogen Peroxide → HCID 13668314, compound

HRID 414669Notes

Reaction equation

HRID 414669 reaction equation
[Cl:1][C:2]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[C:3]=1[C:4]([P:6]([C:15](=[O:24])[C:16]1[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][C:17]=1[Cl:23])[C:7]1[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]=1[CH3:14])=[O:5].[OH:30]O.[PH3]=O>C(#N)C>[Cl:23][C:17]1[CH:18]=[CH:19][CH:20]=[C:21]([Cl:22])[C:16]=1[C:15]([P:6](=[O:30])([C:4](=[O:5])[C:3]1[C:25]([Cl:29])=[CH:26][CH:27]=[CH:28][C:2]=1[Cl:1])[C:7]1[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]=1[CH3:14])=[O:24]

Participants

5

Reactant 3

HCID 784Hydrogen PeroxideHCID 13668313HCID 13668313, compoundHCID 178527022HCID 178527022, compound

Product 1

HCID 13668314HCID 13668314, compoundYield 74%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
60 °C

Procedure

The crude bis-(2,6-dichlorobenzoyl)-2,5-dimethylphenylphosphine (50 grams) is dissolved in 1 liter acetonitrile, mixed with 150 ml of 30% hydrogen peroxide, and heated for one hour at 60° C. The formation of the phosphine oxide is accompanied by deepening of the color, and it precipitates in crystalline form, after the addition of water and cooling. Recrystallization from acetonitrile/water yields 37 grams of the captioned compound (74% of theroretical yield in 2 steps)

Workup

  1. customprecipitates in crystalline form
  2. additionafter the addition of water
  3. temperaturecooling
  4. customRecrystallization from acetonitrile/water

Sources & evidence

ORD record
ord-00ea474f672241fc8634b426b31655c1
Source dataset
uspto-grants-1988_12
Patent number
US04792632

Reaction notes

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