Water → Benzoic acid, 3-sulfo-

HRID 273914

Reaktionsgleichung

Reaktionsgleichung von HRID 273914
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].ClS(C1C=CC=CC=1C(O)=O)(=O)=[O:16].O>C1(C)C(C)=CC=CC=1>[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])([OH:16])(=[O:4])=[O:3]

Komponenten

5

Edukt 3

HCID 962WaterHCID 77641Benzoic acid, 3-(chlorosulfonyl)-HCID 144744642-(Chlorosulfonyl)benzoic acid

Produkt 1

HCID 8477Benzoic acid, 3-sulfo-Ausbeute 95,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

300 g of 3-(chlorosulfonyl)benzoic acid containing 38.8% water (corresponding to 183.6 g (0.83 mol) of 100% chlorosulfonylbenzoic acid) are admixed with 150 g of water and heated at 100° C. for 1 hour. Then 600 g of xylene are added dropwise over 1 hour and a total of 260 ml of water are azeotropically distilled off with xylene. The reaction mixture is cooled and the precipitate is filtered off with suction. After drying at 100° C./100 torr (13.16 kPa) 164.7 g of 3-sulfobenzoic acid are obtained, the purity determined by titration being 97.7%; this corresponds to a yield of 95.6%.

Aufarbeitung

  1. distillationa total of 260 ml of water are azeotropically distilled off with xylene
  2. temperatureThe reaction mixture is cooled
  3. filtrationthe precipitate is filtered off with suction
  4. dry with materialAfter drying at 100° C./100 torr (13.16 kPa) 164.7 g of 3-sulfobenzoic acid
  5. customare obtained

Quellen und Nachweise

ORD-Eintrag
ord-5c21ac4fce2b41ce973bccab5db1a867
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387711

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