反応 #2030163

ord-99fed4c2c183480e86dca7e96e9a731b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was dripped through a dropping funnel into the reaction solution
  2. 2
    その他After the reaction
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    その他the reaction
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    洗浄An organic layer was washed with a sodium hydroxide (NaOH) aqueous solution
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    乾燥a saturated saline solution and dried with magnesium sulfate
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    ろ過After the solution was filtered naturally
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    濃縮the filtrate was concentrated
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    workup.DISSOLUTIONdissolved in toluene
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    ろ過filtered through Florisil, Celite, and alumina
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    濃縮When the filtrate was concentrated
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    その他recrystallized with dichloromethane and hexane, 7.0 g of a light yellow solid of 10-bromo-9-phenylanthracene that
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    その他was obtained (yield: 89%)

実験手順

After 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 dripped through a dropping funnel into the reaction solution. After the dripping, the solution was stirred at room temperature for one hour. After the reaction, a sodium thiosulfate aqueous solution was added to stop the reaction. An organic layer was washed with a sodium hydroxide (NaOH) aqueous solution and a saturated saline solution and dried with magnesium sulfate. After the solution was filtered naturally, the filtrate was concentrated, dissolved in toluene, and filtered through Florisil, Celite, and alumina. When the filtrate was concentrated and recrystallized with dichloromethane and hexane, 7.0 g of a light yellow solid of 10-bromo-9-phenylanthracene that was an object was obtained (yield: 89%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08389735B2uspto-grants-2013_03