反応 #633832

反応方程式

9-phenylanthracene

bromine

sodium thiosulfate

→

9-bromo-10-phenylanthracene

収率 87.4%

溶媒

carbon tetrachloride

carbon tetrachloride

反応条件

後処理

1. 1
   その他A solution obtained
2. 2
   workup.ADDITIONwas dropped into the mixture
3. 3
   その他to be reacted
4. 4
   その他the reaction
5. 5
   洗浄An organic layer of the mixture was washed with water
6. 6
   乾燥dried over magnesium sulfate
7. 7
   ろ過After the drying, the mixture was subjected to suction filtration
8. 8
   その他condensed
9. 9
   その他to obtain a solid
10. 10
    その他The obtained solid was recrystallized by a mixed solvent of chloroform and hexane

実験手順

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).

出典