HRID600103

反应详情

EQUATION

反应方程式

HRID 600103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.0 g (23.7 mmol) of 9-phenylanthracene was dissolved in 80 ml of carbon tetrachloride. A solution of 3.80 g (21.1 mmol) of bromine dissolved in 10 ml of carbon tetrachloride was delivered dropwise into that reaction solution by a dropping funnel. After the dropping was complete, the mixture was stirred for 1 hour at room temperature. After the reaction, a sodium thiosulfate solution was added to stop the reaction. An organic layer was washed with a NaOH solution and a saturated saline solution, and dried with magnesium sulfate. After natural filtration, concentration and dissolving in toluene were conducted. Then, filtration was done through Florisil, Celite and alumina. The filtrate was concentrated, then recrystallized with dichloromethane and hexane. The target substance, 9-bromo-10-phenylanthracene, was obtained in the form of a pale yellow solid, weighing 7.0 g in a yield of 89% (synthesis scheme (j-4)).

WORKUP

后处理

  1. customwas delivered dropwise into that reaction solution by a dropping funnel
  2. customAfter the reaction
  3. customthe reaction
  4. washAn organic layer was washed with a NaOH solution
  5. dry with materiala saturated saline solution, and dried with magnesium sulfate
  6. filtrationAfter natural filtration, concentration
  7. dissolutiondissolving in toluene
  8. filtrationThen, filtration
  9. concentrationThe filtrate was concentrated
  10. customrecrystallized with dichloromethane and hexane