반응 #1248165

반응 방정식

9-phenylanthracene

bromine

sodium thiosulfate

→

9-bromo-10-phenylanthracene

수율 89.0%

용매

carbon tetrachloride

carbon tetrachloride

반응 조건

후처리

1. 1
   기타was delivered dropwise into that reaction solution by a dropping funnel
2. 2
   기타After the reaction
3. 3
   기타the reaction
4. 4
   세척An organic layer was washed with a NaOH solution
5. 5
   건조a saturated saline solution, and dried with magnesium sulfate
6. 6
   여과After natural filtration, concentration
7. 7
   workup.DISSOLUTIONdissolving in toluene
8. 8
   여과Then, filtration
9. 9
   농축The filtrate was concentrated
10. 10
    기타recrystallized with dichloromethane and hexane

실험 절차

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)).

출처