Hydrogen Peroxide → 3-Sulphoperoxybenzoic acid

HRID 485216

Reaktionsgleichung

Reaktionsgleichung von HRID 485216
[S:1]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])([OH:4])(=[O:3])=[O:2].[OH:14]O>ClCCl.S(=O)(=O)(O)O>[S:1]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([O:10][OH:14])=[O:9])([OH:4])(=[O:3])=[O:2]

Komponenten

5

Edukt 2

HCID 784Hydrogen PeroxideHCID 8477Benzoic acid, 3-sulfo-

Produkt 1

HCID 98158233-Sulphoperoxybenzoic acidAusbeute 64,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1118Sulfuric AcidKatalysatorHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
42 °C

Versuchsvorschrift

To a suspension of 3-sulphobenzoic acid (5 g, 2.5×10-2 moles) in dichloromethane (60 ml) containing a trace of sulphuric acid (5×10-5 moles) was slowly added hydrogen peroxide (3 g; 85%). The suspension was boiled under reflux (42° C.) for 1 hour after which it was cooled to room temperature, the dichloromethane was decanted off and the residue treated with saturated aqueous magnesium nitrate (25 ml). The resultant precipitate was filtered off, dried over phosphorous pentoxide under vacuum to yield the magnesium salt of 3-sulphoperoxybenzoic acid (3.5 g; 5.31% Avox as O; Magnesium content of 4.7%) compared with a theoretical yield of 5.67 g. The IR spectrum was again substantially the same as for the other preparations.

Aufarbeitung

  1. temperaturewas cooled to room temperature
  2. customthe dichloromethane was decanted off
  3. additionthe residue treated with saturated aqueous magnesium nitrate (25 ml)
  4. filtrationThe resultant precipitate was filtered off
  5. dry with materialdried over phosphorous pentoxide under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-0cff83a548e745d9ac7dc42b94745dbf
Quelldatensatz
uspto-grants-1985_08
Patentnummer
US04536313

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