Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Toluene | HCID 1140 | — |
| Edukt | Dichlorodimethylsilane | HCID 6398 | — |
| Edukt | 1H-Indene, 2-methyl- | HCID 16587 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Dimethyl-bis(2-methyl-1H-inden-1-yl)silane | HCID 4050248 | — |
Reaktionsschritte
8.0 g (61.4 mmoles) of 2-methylindene were introduced into 175 mL of toluene and 13 mL of THF, and 24.6 mL of n-butyllithium (2.5 Min toluene) were added without interruption at room temperature. After this addition was complete, the mixture was heated to 80° C. and stirred at this temperature for one hour. It was allowed to cool to 40° C., then 3.96 g (30.7 mmoles) of dimethyldichlorosilane were slowly added dropwise. After this addition, the reaction solution was stirred for three hours at 60° C. and then overnight at room temperature. 70 mL of water were added and the phases that form were separated. The organic phase was washed with 100 mL of water, and the aqueous phase was extracted three times with a total of 100 mL of toluene. The combined organic phases were dried over magnesium sulfate. After separation of the magnesium sulfate, the solvent was removed and the residue was purified by column chromatography. The desired product was isolated in a yield of 8.16 g (84%) (purity 99%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08299287B2 |
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| Quelldatensatz | uspto-grants-2012_10 |
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| ORD ID | ord-e578723e9e7f4039a4b6fadaa31fb67f |
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| Quellennotiz | uspto-grants-2012_10 |
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