Реакция #885
ord-bfcf42b524d14d69860f018538be3094
Уравнение реакции
9,9-bis(4-hydroxyphenyl)fluorene
ethylene carbonate
potassium carbonate
18-crown-6
→
white powder
4-(2-hydroxyethoxyphenyl)fluorene
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураat reflux
- 2Другоеthe solvent was decanted from the precipitated product
- 3ПромывкаThe resulting white solid was washed with ligroin (
- 4Другоеdried under a stream of nitrogen
- 5ДругоеThe product was recrystallized from methanol
Методика
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.