HRID1770298

反应详情

EQUATION

反应方程式

HRID 1770298 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 (3.5 g, 10 mmol) and 40 ml of acetic acid was stirred and then 4-nitrophthalic anhydride (4.1 g, 21 mmol) was added to the mixture. The resulting mixture was stirred and heated under reflux for 7 hours. After cooling, the beige-colored precipitate was filtered, washed with acetic acid (2×100 ml) and then with water (500 ml). The washed precipitate was recrystallized from dimethyl-fromamide-methanol to provide the title compound as an off-white powder (5.1 g, 73% yield) having a melting point of 360°-363° C.

WORKUP

后处理

  1. stirringThe resulting mixture was stirred
  2. temperatureheated
  3. temperatureunder reflux for 7 hours
  4. temperatureAfter cooling
  5. filtrationthe beige-colored precipitate was filtered
  6. washwashed with acetic acid (2×100 ml)
  7. customThe washed precipitate was recrystallized from dimethyl-fromamide-methanol