반응 #633832

반응 방정식

9-phenylanthracene

bromine

sodium thiosulfate

→

9-bromo-10-phenylanthracene

수율 87.4%

용매

carbon tetrachloride

carbon tetrachloride

반응 조건

후처리

1. 1
   기타A solution obtained
2. 2
   workup.ADDITIONwas dropped into the mixture
3. 3
   기타to be reacted
4. 4
   기타the reaction
5. 5
   세척An organic layer of the mixture was washed with water
6. 6
   건조dried over magnesium sulfate
7. 7
   여과After the drying, the mixture was subjected to suction filtration
8. 8
   기타condensed
9. 9
   기타to obtain a solid
10. 10
    기타The obtained solid was recrystallized by a mixed solvent of chloroform and hexane

실험 절차

20.8 g (81.7 mmol) of 9-phenylanthracene and 300 mL of carbon tetrachloride were put into a 500 mL three-necked flask. A solution obtained by dissolving 13.1 g (81.7 mmol) of bromine in 5.00 mL of carbon tetrachloride was dropped into the mixture. After the dropping was completed, the reaction solution was stirred at room temperature for 3 hours to be reacted. Then, about 100 mL of a sodium thiosulfate solution was added to the reaction solution to complete the reaction. An organic layer of the mixture was washed with water and dried over magnesium sulfate. After the drying, the mixture was subjected to suction filtration, and the filtrate was condensed to obtain a solid. The obtained solid was recrystallized by a mixed solvent of chloroform and hexane; then 23.8 g of objective 9-bromo-10-phenylanthracene was obtained as a light yellow powdered solid in a yield of 71%. A synthetic scheme of 9-bromo-10-phenylanthracene is illustrated below (synthetic scheme b-2).

출처