反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
The monomer 4,4'-bis(1-naphthoxy)octafluorobiphenyl (8FNE) was prepared by the following procedure. A 100 mL round bottom flask was charged with decafluorobiphenyl (3.01 g, 0.0090 mole), 1-naphthol (2.60 g, 0.0181 mole), potassium carbonate (2.95 g, 0.0218 mole), and DMAc (40 g). The mixture was heated with stirring at about 140° C. for 2 hr and then cooled to room temperature, filtered, and poured into toluene (100 mL). The toluene solution was washed with 5% sodium hydroxide (50 mL) and then twice with deionized water (2×100 mL). After drying with magnesium sulfate and filtering, it was concentrated by rotary evaporation to yield a red solid. The solid was recrystallized from DMAc/water, filtered, and dried to yield 8FNE (3.9 g, 78.8% yield; m.p. 189°-191 ° C.; GC/MS m+ /e 582).
WORKUP
后处理
- temperatureThe mixture was heated
- temperaturecooled to room temperature
- filtrationfiltered
- additionpoured into toluene (100 mL)
- washThe toluene solution was washed with 5% sodium hydroxide (50 mL)
- dry with materialAfter drying with magnesium sulfate
- filtrationfiltering
- concentrationit was concentrated by rotary evaporation
- customto yield a red solid
- customThe solid was recrystallized from DMAc/water
- filtrationfiltered
- customdried
- customto yield 8FNE (3.9 g, 78.8% yield; m.p. 189°-191 ° C.; GC/MS m+ /e 582)