참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | 3,6-DI-Tert-butylfluorene | HCID 11140437 | — |
| 반응물 | 2-tert-Butyl-5-(propan-2-ylidene)cyclopenta-1,3-diene | HCID 14688283 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-(3-Tert-butylcyclopentadienyl)-2-(3,6-di-tert-butylfluorenyl)propane | HCID 131725121 | 43.1% |
반응 단계
To a solution of 1.98 g (7.1 mmol) of 3,6-di-tert-butylfluorene in 40 ml of ether, 4.6 ml (7.5 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 1.56 g (9.6 mmol) of 3-tert-butyl-6,6-dimethylfulvene in 20 ml of ether was further dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. Then, 60 ml of water was added. The separated organic phase was dried over magnesium sulfate and then filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a solid. The solid was purified by column chromatography (silica gel, developing solvent: hexane) to obtain 1.35 g of a light yellow solid (yield: 43%). The analyzed values are given below.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07449533B2 |
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| 출처 데이터셋 | uspto-grants-2008_11 |
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| ORD ID | ord-b6650b087f9742b3899941e4f6965496 |
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| 출처 메모 | uspto-grants-2008_11 |
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