HRID1770298
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
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
- stirringThe resulting mixture was stirred
- temperatureheated
- temperatureunder reflux for 7 hours
- temperatureAfter cooling
- filtrationthe beige-colored precipitate was filtered
- washwashed with acetic acid (2×100 ml)
- customThe washed precipitate was recrystallized from dimethyl-fromamide-methanol