반응 #885

반응 방정식

9,9-bis(4-hydroxyphenyl)fluorene

ethylene carbonate

potassium carbonate

18-crown-6

→

white powder

4-(2-hydroxyethoxyphenyl)fluorene

용매

반응 조건

후처리

1. 1
   온도at reflux
2. 2
   기타the solvent was decanted from the precipitated product
3. 3
   세척The resulting white solid was washed with ligroin (
4. 4
   기타dried under a stream of nitrogen
5. 5
   기타The product was recrystallized from methanol

실험 절차

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.

출처