Hydrogen Peroxide → Diperoxy trimellitic acid

HRID 36542

Reaktionsgleichung

Reaktionsgleichung von HRID 36542
[CH:1]1[C:6]([C:7](O)=[O:8])=[CH:5]C2C([O:12][C:13](=[O:14])[C:3]=2[CH:2]=1)=O.S(=O)(=O)(O)[OH:16].[OH:20][OH:21].[C:22]([O:25]CC)(=[O:24])[CH3:23]>CS(O)(=O)=O>[C:13]([O:12][OH:16])(=[O:14])[C:3]1[C:23](=[CH:5][C:6](=[CH:1][CH:2]=1)[C:7]([O:20][OH:21])=[O:8])[C:22]([OH:25])=[O:24]

Komponenten

6

Edukt 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 8857Ethyl AcetateHCID 11089Trimellitic anhydride

Produkt 1

HCID 131718999Diperoxy trimellitic acidAusbeute 70,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6395Methanesulfonic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
15 °C

Versuchsvorschrift

4.00 g (0.0221 mol) trimellitic acid anhydride was dissolved in 60 ml 98% methane-sulfonic acid and 20 ml 98% sulfuric acid during 1 hour at 40° C. and was then cooled to 15° C. 4.99 g (0.125 mol) 85% hydrogen peroxide was added by drops during 15 minutes. After 2 hours at 30° C. the mixture was cooled and gently poured into 800 ml ice-cold (0°-10° C.) ethyl acetate under agitation, whereupon 200 ml saturated (NH4)2SO4 solution was added. After 2 hours vigorous agitation the ethyl acetate phase was separated and dried over Na2SO4. The ethyl acetate was evaporated until a viscous yellow-white oil remained. Diperoxy trimellitic acid crystallized in petroleum-ether/diethylether and was dried until constant weight. Titration on active oxygen showed a yield of 70.7%.

Aufarbeitung

  1. temperatureAfter 2 hours at 30° C. the mixture was cooled
  2. additionwas added
  3. customAfter 2 hours vigorous agitation the ethyl acetate phase was separated
  4. dry with materialdried over Na2SO4
  5. customThe ethyl acetate was evaporated until a viscous yellow-white oil
  6. customDiperoxy trimellitic acid crystallized in petroleum-ether/diethylether
  7. customwas dried until constant weight

Quellen und Nachweise

ORD-Eintrag
ord-9bc279c838d24e0485307713cc7423f3
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05415668

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