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-(1,1-Dimethylpropyl)-6,6-dimethylfulvene | HCID 17818147 | — |
| 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 | 1-(3-(1,1-Dimethylpropyl)cyclopentadienyl)-1-(3,6-di-tert-butylfluorenyl)cyclohexane | HCID 131725141 | 45% |
反応手順
To a solution of 2.38 g (8.5 mmol) of 3,6-di-tert-butylfluorene in 40 ml of THF, 5.7 ml (9.2 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 (9.2 mmol) of 3-(1,1-dimethylpropyl)-6,6-dimethylfulvene in 30 ml of THF was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. 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 1.88 g (3.80 mmol) of a white solid (yield: 45%). 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-5375b988de2d4f0699d927681af91b4e |
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| 出典メモ | uspto-grants-2008_11 |
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