HRID1031052

反应详情

EQUATION

反应方程式

HRID 1031052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

The monomer 1,4-bis(1-naphthoxy)tetrafluorobenzene (4FNE) was prepared as follows. A 100 mL round bottom flask equipped with a magnetic stirrer was charged with hexafluorobenzene (3.53 g, 0.0190 mole), 1-naphthol, and DMAc (50 mL). After the solids dissolved, potassium carbonate (6.50 g, 0.048 mole) was added and the mixture was heated at about 140° C. for 2 hr. The mixture was then cooled to room temperature, filtered, and poured into toluene (150 mL). The toluene solution was washed twice with water (2×150 mL) and concentrated by rotary evaporation to yield an off-white powder (7.91 g). Analysis of the powder by GC showed a mixture of isomers (2% ortho, 8% meta, and 90% para). The powder was recrystallized from a mixture of N,N-dimethylformamide (DMF) and water to yield the desired all-para 4FNE, GC/MS (m+ /e 434).

WORKUP

后处理

  1. customA 100 mL round bottom flask equipped with a magnetic stirrer
  2. dissolutionAfter the solids dissolved
  3. temperatureThe mixture was then cooled to room temperature
  4. filtrationfiltered
  5. additionpoured into toluene (150 mL)
  6. washThe toluene solution was washed twice with water (2×150 mL)
  7. concentrationconcentrated by rotary evaporation