참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Dimethyl-bis(2-methyl-1H-inden-1-yl)silane | HCID 4050248 | — |
| 반응물 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178421900 | HCID 178421900 | 35% |
반응 단계
15.3 ml (38.4 mmol) of a 2.5 molar solution of buthyllithium hexane were added to a solution of 6.07 g (19.2 mmol) dimethylbis(2-methylindenyl)-silane in 80 ml tetrahydrofuran. The mixture was refluxed for 2 hours prior to solvent evaporation. The residue was suspended in 30 ml of hexane, the suspension was filtrated and the dilithio-compound was dried in vacuo. The dilithio-compound was then added to a suspension of 4.47 g (19.2 mmol) zirconiumtetrachloride in 50 ml metylenchloride at -78° C. The suspension was slowly warmed to room temperature and stirred over night. The suspension was filtrated and the meso-compound was removed by extraction with toluene. The residue was extracted with 70 ml methylenchloride, the filtrat was concentrated and stored for crystallisation at -30° C. Filtration of the suspension afforded 3,20 g (35%) rac-dimethylsilandiylbis(2-methylindenyl)zirconocen dichloride.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05831105 |
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| 출처 데이터셋 | uspto-grants-1998_11 |
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| ORD ID | ord-b1d0fa4901ef4ca39ca00bbaa9d3809a |
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| 출처 메모 | uspto-grants-1998_11 |
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