HRID7194

反应详情

EQUATION

反应方程式

HRID 7194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1.2 litters of propylene carbonate and 160 g (0.96 mol) of fluorene were put into a 2 litter 3-neck round-bottom flask equipped with a stirrer, a thermometer and a reflux condenser under an argon atmosphere, and the resulting mixture was heated to 80° C. so as to make completely dissolved. 179.9 g (1.01 mol) of N-bromosuccinimide was added portionwise to the reaction mixture, and the resultant was stirred at 80° C. for 10 hours. The reaction mixture was cooled down to room temperature to precipitate white solid. The solid was filtered, thoroughly washed with methanol, dried and then recrystallized from ethanol, to obtain white crystal, which was filtered and then sufficiently dried in a vacuum oven at 40° C. to give 160 g (yield: 60%) of the desired product, and its melting point was 102° C.–103° C.

WORKUP

后处理

  1. customequipped with a stirrer
  2. dissolutionto make completely dissolved
  3. temperatureThe reaction mixture was cooled down to room temperature
  4. customto precipitate white solid
  5. filtrationThe solid was filtered
  6. washthoroughly washed with methanol
  7. customdried
  8. customrecrystallized from ethanol
  9. customto obtain white crystal, which
  10. filtrationwas filtered
  11. customsufficiently dried in a vacuum oven at 40° C.