関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 9-Phenylanthracene | HCID 11766 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 9-Bromo-10-phenyl-anthracene | HCID 4155836 | 89% |
反応手順
6.0 g (23.7 mmol) of 9-phenylanthracene was dissolved in 80 mL of carbon tetrachloride, and then, in the reaction solution thereof, a solution in which 3.80 g (21.1 mmol) of bromine was dissolved in 10 mL of carbon tetrachloride was dropped by a dropping funnel. After dropping, it was stirred for one hour at room temperature. After reaction, a sodium thiosulfate aqueous solution was added thereto and stirred. An organic layer was washed with a sodium hydroxide aqueous solution and saturated saline, and then dried with magnesium sulfate. After the mixture was subjected to natural filtration, the filtrate was concentrated and dissolved in toluene, and then filtration was carried out using florisil, celite, and alumina. When the filtrate was concentrated and then recrystallized with a mixed solution of dichloromethane and hexane, 7.0 g of 9-bromo-10-phenylanthracene that was a target substance was obtained as a light yellow solid at a yield of 89% (Synthesis scheme (b-2)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08860019B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-7b6fe09197b24aeeb27eeba13a29b3e4 |
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| 出典メモ | uspto-grants-2014_10 |
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