Reaktion #361341

Reaktionsgleichung

4-hydroxy-4'-octyloxybiphenyl

NaOH

chlorodifluoromethane

→

4-Difluoromethoxy-4'-octoxy-biphenyl

Lösungsmittel

water

dioxane

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe product is extracted with petroleum ether
2. 2
   TrocknenThe organic phase is dried over Na2SO4
3. 3
   Sonstigeevaporated
4. 4
   Filtrationthe residue is filtered through a short silica gel column
5. 5
   SonstigeThe product is recrystallized from acetonitrile
6. 6
   SonstigeColourless crystals are obtained
7. 7
   Sonstige20° C. (extrapolated), Δn =0.093, viscosity

Vorschrift

A mixture of 20 g of 4-hydroxy-4'-octyloxybiphenyl, 13.6 g of NaOH, 100 ml of water and 150 ml of dioxane is heated to 70° C. with stirring. 10 g of chlorodifluoromethane are passed into the cooled two-phase mixture with vigorous stirring. The reaction mixture is poured into water, and the product is extracted with petroleum ether. The organic phase is dried over Na2SO4, evaporated, and the residue is filtered through a short silica gel column using petroleum ether as eluent. The product is recrystallized from acetonitrile. Colourless crystals are obtained. m.p.: 104° C., c.p.: 20° C. (extrapolated), Δn =0.093, viscosity: 17

Quelle