関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 3,6-DI-Tert-butylfluorene | HCID 11140437 | — |
| 反応物 | 3-(1-Methyl-1-cyclohexyl)-6,6-dimethylfulvene | HCID 14688282 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(3-(1-Methyl-1-cyclohexyl)cyclopentadienyl)-2-(3,6-di-tert-butylfluorenyl)propane | HCID 131725122 | 43% |
反応手順
To a solution of 2.64 g (9.5 mmol) of 3,6-di-tert-butylfluorene in 45 ml of THF, 6.4 ml (10.4 mmol) of a hexane solution of n-butyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. To the resulting red solution, a solution of 2.00 g (9.9 mmol) of 3-(1-methyl-1-cyclohexyl)-6,6-dimethylfulvene in 30 ml of THF was further dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for 3 days. After the reaction solution was diluted with 100 ml of ether, 50 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was isolated and purified by column chromatography (silica gel, developing solvent: hexane) to obtain 1.96 g (4.08 mmol) of a white solid (yield: 43%). The analyzed values are given below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449533B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-6dca80c9b37e4cabb8f68954b6386527 |
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| 出典メモ | uspto-grants-2008_11 |
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