Reaktion #416938

Reaktionsgleichung

o-phenylphenol

sulfuric acid

→

product

Ausbeute 85.0%

bis(3-phenyl-4-hydroxyphenyl)sulfone

Ausbeute 85.0%

Lösungsmittel

chlorobenzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   workup.DISTILLATIONWhile the generated water was distilled away with chlorobenzene
3. 3
   Temperaturthe organic phase of the distillate was refluxed into the reaction vessel
4. 4
   Sonstigerose to 165° C.
5. 5
   Temperaturthe reaction mixture was cooled
6. 6
   workup.ADDITIONby adding 500 milliliters of xylene
7. 7
   Sonstigeto precipitate crystals
8. 8
   SonstigeThe crystals were recrystallized from acetone-cyclohexane mixture solution

Vorschrift

To a mixture of 391 g (2.3 mol) of o-phenylphenol, 100 g (1 mol) of 98% by weight sulfuric acid, and 100 g of chlorobenzene was added 9.5 g (0.05 mol) of benzenesulfonic acid and heated with stirring. While the generated water was distilled away with chlorobenzene and the organic phase of the distillate was refluxed into the reaction vessel, the reaction was carried out for 10 hours. At the time when the distilled water amounted to 36 milliliters and the temperature in the reaction vessel rose to 165° C., the reaction mixture was cooled by adding 500 milliliters of xylene to precipitate crystals. The crystals were recrystallized from acetone-cyclohexane mixture solution to obtain 340 g of a product (yield: 85%). The melting point of the product was between 251° to 252° C. and the results of 1H-NMR (acetone d6) were as follows.

Quelle