Reaktion #885

Reaktionsgleichung

9,9-bis(4-hydroxyphenyl)fluorene

ethylene carbonate

potassium carbonate

18-crown-6

→

white powder

4-(2-hydroxyethoxyphenyl)fluorene

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux
2. 2
   Sonstigethe solvent was decanted from the precipitated product
3. 3
   WaschenThe resulting white solid was washed with ligroin (
4. 4
   Sonstigedried under a stream of nitrogen
5. 5
   SonstigeThe product was recrystallized from methanol

Vorschrift

A mixture of 84.4 g (0.241 mol) of 9,9-bis(4-hydroxyphenyl)fluorene, 46.7 g (0.53 mol) of ethylene carbonate, 3.3 g (0.024 mol) of potassium carbonate, and a catalytic amount of 18-crown-6 in 400 mL of xylenes was heated at reflux with mechanical stirring for 6 h. The mixture was allowed to cool slowly to room temperature, and the solvent was decanted from the precipitated product. The resulting white solid was washed with ligroin (to prevent the formation of a gummy mass), and dried under a stream of nitrogen. The product was recrystallized from methanol, providing 70.4 g (67%) of a white powder.

Quelle