Water → 2-Phenylsulphenyl-4-trifluoromethylbenzoic acid

HRID 1491575Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1491575
[C:1]1([S:7][C:8]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[CH:12][C:9]=2[C:10]#N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)[OH:21].[OH2:25]>>[C:1]1([S:7][C:8]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[CH:12][C:9]=2[C:10]([OH:21])=[O:25])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 3

HCID 962Water2×HCID 1118Sulfuric AcidHCID 189779842-Phenylsulphenyl-4-trifluoromethylbenzonitrile

Produkt 1

HCID 189779402-Phenylsulphenyl-4-trifluoromethylbenzoic acid

Versuchsvorschrift

A mixture of 2-phenylsulphenyl-4-trifluoromethylbenzonitrile (9 g), concentrated sulphuric acid (27 ml) and water was heated at reflux for 10 hours. The mixture was then cooled, poured into water and extracted with dichloromethane. The organic extract was extracted with aqueous sodium hydroxide. The resulting aqueous solution was acidified with aqueous hydrochloric acid to pH 1. The suspension was extracted with dichloromethane, dried over anhydrous sodium sulphate, filtered and after evaporation of the dichloromethane, 2-phenylsulphenyl-4-trifluoromethylbenzoic acid was obtained as a white solid (7.5 g), m.p. 161° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 10 hours
  3. temperatureThe mixture was then cooled
  4. extractionextracted with dichloromethane
  5. extractionThe organic extract
  6. extractionwas extracted with aqueous sodium hydroxide
  7. extractionThe suspension was extracted with dichloromethane
  8. dry with materialdried over anhydrous sodium sulphate
  9. filtrationfiltered
  10. customafter evaporation of the dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-65f17692cb1448c78b8946090439eedb
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05371064

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