関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,7-Dibromo-9-fluorenone | HCID 259922 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 9-(2-Biphenylyl)-2,7-dibromo-9-fluorenol | HCID 22016047 | 198.7% |
反応手順
15.2 g (45 mmol) of 2,7-dibromo-9-fluorenone was put in a 100 mL three-necked flask, and nitrogen substitution was conducted. 40 mL of diethyl ether was added. The Grignard reagent above was transferred into a dropping funnel by a cannula so as not to expose it to the atmosphere, and was added dropwise into the mixture. The mixture was refluxed at 50° C. After the reaction, the solution was washed with water. Then the aqueous layer was extracted with ethyl acetate and combined with the organic layer. The layers were washed with a saturated saline solution, then dried with magnesium sulfate. Filtration and concentration were carried out, and 22 g of 9-(biphenyl-2-yl)-2,7-dibromo-9-fluorenol was obtained as a white solid, in a yield of 90%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07897964B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-7644fd9bc8b649949e93ad86085126fa |
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| 出典メモ | uspto-grants-2011_03 |
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