Hydrogen Peroxide → Monoperoxyphthalic acid

HRID 719846

Reaktionsgleichung

Reaktionsgleichung von HRID 719846
C([O-])([O-])=O.[Na+].[Na+].[OH:7][OH:8].[C:9]1(=[O:19])[O:14][C:12](=[O:13])[C:11]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:10]12.OS(O)(=O)=O>O>[CH:17]1[CH:18]=[C:10]([C:9]([OH:14])=[O:19])[C:11]([C:12]([O:7][OH:8])=[O:13])=[CH:15][CH:16]=1

Komponenten

6

Edukt 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 6811Phthalic AnhydrideHCID 10340Sodium Carbonate

Produkt 1

HCID 75329Monoperoxyphthalic acidAusbeute 76,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

Deionized water (125 ml), Na2CO3 (31.0 g, 0.25 mol) and 35% H2O2 (29.15 g, 0.3 mol) are successively charged in a 500 ml four-neck flask, and the mixture was stirred in a dry ice-methanol bath at −5° C.–0° C. Thereto was added phthalic anhydride (37.0 g, 0.25 mol) and the mixture was stirred for 30 min. The bath was removed, ethyl acetate (100 ml) was added to the mixture, and the reaction system was neutralized in a solution obtained by diluting 98% H2SO4 (15 ml) with deionized water (50 ml). After partitioning, the aqueous layer was extracted with ethyl acetate (60 ml). The obtained organic layer (0.64 g) was taken up and saturated NaI-IPA (isopropyl alcohol) solution (5 ml) and 10% acetic acid-IPA solution (20 ml) were added thereto. The mixture was boiled for 5 min. It was titrated with 0.1N aqueous sodium thiosulfate solution. As a result, mono-perphthalic acid was present in 33.5 g and the yield was 76.9%.

Aufarbeitung

  1. stirringthe mixture was stirred for 30 min
  2. customThe bath was removed
  3. additionethyl acetate (100 ml) was added to the mixture
  4. customobtained
  5. customAfter partitioning
  6. extractionthe aqueous layer was extracted with ethyl acetate (60 ml)
  7. additionsaturated NaI-IPA (isopropyl alcohol) solution (5 ml) and 10% acetic acid-IPA solution (20 ml) were added

Quellen und Nachweise

ORD-Eintrag
ord-ad9fdcc6fe6045d58fb91747ed8a1665
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07132560B2

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