反応 #687285

反応方程式

9-phenylanthracene

bromine

sodium thiosulfate

→

9-bromo-10-phenylanthracene

収率 89.0%

溶媒

carbon tetrachloride

carbon tetrachloride

反応条件

後処理

1. 1
   その他was delivered dropwise into that reaction solution by a dropping funnel
2. 2
   その他After the reaction
3. 3
   その他the reaction
4. 4
   洗浄An organic layer was washed with a NaOH solution
5. 5
   乾燥a saturated saline solution, and dried with magnesium sulfate
6. 6
   ろ過After natural filtration, concentration
7. 7
   workup.DISSOLUTIONdissolving in toluene
8. 8
   ろ過Then, filtration
9. 9
   濃縮The filtrate was concentrated
10. 10
    その他recrystallized with dichloromethane and hexane

実験手順

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)).

出典