HRID1770295

反应详情

EQUATION

反应方程式

HRID 1770295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9,9-bis(4-aminophenyl )fluorene (17.4 g, 50 mmol), 4-fluorophthalic anhydride (18.3 g, 110 mmol), and 250 ml of acetic acid was stirred and heated under reflux for five hours and then stirred at ambient temperature overnight. A colorless precipitate formed which was filtered, washed twice with 150 ml of ethanol, washed twice with 100 ml of hexane, suction-dried for two hours, and then dried in a vacuum oven at 120° C. for 16 hours. The title compound was isolated as a colorless powder (29.2 g, 90.6% yield) that had melting point of 323.5°-326° C. and a 1H NMR spectrum (DMSO-d6) corresponding to δ8.02 (m, 4H), 7.86 (dd, 2H), 7.72 (m, 2H), 7.60 (d, 2H), 7.46 (t, 2H), and 7.35 (m, 10H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for five hours
  3. stirringstirred at ambient temperature overnight
  4. customA colorless precipitate formed which
  5. filtrationwas filtered
  6. washwashed twice with 150 ml of ethanol
  7. washwashed twice with 100 ml of hexane
  8. customsuction-dried for two hours
  9. customdried in a vacuum oven at 120° C. for 16 hours