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 | 2-(3-(1,1-Dimethylpropyl)cyclopentadienyl)-2-(3,6-di-tert-butylfluorenyl)propane | HCID 131725126 | 59% |
反応手順
To a solution of 2.14 g (7.7 mmol) of 3,6-di-tert-butylfluorene in 40 ml of THF, 5.0 ml (8.1 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 1.81 g (10.3 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 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 2.06 g (4.53 mmbl) of a white solid (yield: 59%). 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-7eace6301274482588a0215787328afc |
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| 出典メモ | uspto-grants-2008_11 |
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