反応 #885

反応方程式

9,9-bis(4-hydroxyphenyl)fluorene

ethylene carbonate

potassium carbonate

18-crown-6

→

white powder

4-(2-hydroxyethoxyphenyl)fluorene

溶媒

反応条件

後処理

1. 1
   温度at reflux
2. 2
   その他the solvent was decanted from the precipitated product
3. 3
   洗浄The resulting white solid was washed with ligroin (
4. 4
   その他dried under a stream of nitrogen
5. 5
   その他The product was recrystallized from methanol

実験手順

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.

出典