反応 #2013361

反応方程式

9-phenylanthracene

bromine

sodium thiosulfate

→

10-bromo-9-phenylanthracene

収率 99.6%

溶媒

carbon tetrachloride

carbon tetrachloride

反応条件

後処理

1. 1
   workup.ADDITIONwas dropped into the reaction solution
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 an aqueous sodium hydroxide (NaOH) solution
5. 5
   乾燥a saturated sodium chloride solution and dried with magnesium sulfate
6. 6
   ろ過The mixture was naturally filtered
7. 7
   その他a compound obtained
8. 8
   濃縮by concentrating the filtrate
9. 9
   workup.DISSOLUTIONwas dissolved into toluene
10. 10
    ろ過filtered through florisil, Celite®, and alumina
11. 11
    濃縮The filtrate was concentrated
12. 12
    その他recrystallized with dichloromethane and hexane

実験手順

6.0 g (23.7 mmol) of 9-phenylanthracene was dissolved into 80 mL of carbon tetrachloride, and a solution in which 3.80 g (21.1 mmol) of bromine was dissolved in 10 mL of carbon tetrachloride was dropped into the reaction solution using a dropping funnel. After dropping, the solution was stirred for 1 hour at a room temperature. After the reaction, an aqueous sodium thiosulfate solution was added to stop the reaction. An organic layer was washed with an aqueous sodium hydroxide (NaOH) solution and a saturated sodium chloride solution and dried with magnesium sulfate. The mixture was naturally filtered, and a compound obtained by concentrating the filtrate was dissolved into toluene and filtered through florisil, Celite®, and alumina. The filtrate was concentrated and recrystallized with dichloromethane and hexane, thereby obtaining 7.0 g of objective 10-bromo-9-phenylanthracene as a light-yellow solid with a yield of 89%.

出典