関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4,7-dimethyl-1H-indene | HCID 81458 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Tetrahydrofuran hexane | HCID 21883165 | — |
| 生成物 | 1-(4,7-Dimethyl-1-indenyl)-2-(4,7-dimethyl-1-indenyl)methyl benzene | HCID 18471716 | — |
反応手順
4.12 ml (10.3 mmoles) of n-BuLi 2.5 M in hexane are added to a solution of 1.48 g of 4,7-dimethyl indene (XVIII) (10.3 mmoles; obtained as described above) in 55 ml of a mixture of THF-hexane 2/1. At the end of the addition, the mixture is left under stirring for 1 hour. It is then cooled to −70° C. and a solution of 2.3 g of the brominated compound having formula (XX) (7.37 mmoles) in THF/hexane are added dropwise. The mixture is left to rise to room temperature and is left to rest for 6 hours. It is then poured into water and is extracted with ethyl ether. The organic phase is washed until neutrality and dehydrated on sodium sulfate. The residue obtained by evaporation of the solvent is purified by silica gel chromatography eluating with petroleum ether. After evaporation of the eluant 2.0 g of the bis-indenyl ligand having formula (XXI) and indicated below, are obtained (72% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211110B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-5126c223f2b14f7bab136e8816d4a689 |
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| 出典メモ | uspto-grants-2001_04 |
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