Sodium Hydroxide → Sodium 4-(trifluoromethoxy)benzenesulfonate

HRID 469135

Reaktionsgleichung

Reaktionsgleichung von HRID 469135
[F:1][C:2]([F:11])([F:10])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[OH:12][S:13](O)(=[O:15])=[O:14].O=S(=O)=O.[OH-].[Na+:22]>>[F:1][C:2]([F:10])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([S:13]([O-:15])(=[O:14])=[O:12])=[CH:6][CH:5]=1.[Na+:22]

Komponenten

4

Edukt 3

HCID 14798Sodium HydroxideHCID 24681Fuming sulfuric acidHCID 68010(Trifluoromethoxy)benzene

Produkt 1

HCID 89511132Sodium 4-(trifluoromethoxy)benzenesulfonateAusbeute 24 %

Versuchsvorschrift

A 100 mL flask equipped with a stir-bar and a nitrogen bubbler was charged with (trifluoromethoxy)-benzene (5.015 g) at room temperature. Oleum (15% SO3, 9.30 g) was added to the above flask at 10° C. The reaction mixture was allowed to warm to room temperature and stirred at room temperature for 15 h. A sodium hydroxide solution (7.75 g, in 23 mL water) was slowly added to the reaction mixture while the reaction mixture was cooled with an ice-water bath. The resulting solid was collected by filtration, dried under vacuum, and then extracted with refluxing ethanol. The ethanol solution was dried to give sodium 4-(trifluoromethoxy)benzenesulfonate (3FMBSNa) 2.0 g (yield 24%): 1H NMR (D2O) 7.45 (d, J=9 Hz, 2H), 7.89 (m, 2H) ppm; 19F NMR (D2O)-58.1 (s) ppm.

Aufarbeitung

  1. customA 100 mL flask equipped with a stir-bar
  2. temperaturewas cooled with an ice-water bath
  3. filtrationThe resulting solid was collected by filtration
  4. customdried under vacuum
  5. extractionextracted with refluxing ethanol
  6. dry with materialThe ethanol solution was dried

Quellen und Nachweise

ORD-Eintrag
ord-997842f8c1d54d878c1a82838cad9e3e
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08628682B2

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