Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Imidazole | HCID 795 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | 3,5-Dimethoxyphenol | HCID 10383 | — |
| Edukt | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-t-Butyldiphenylsiloxy-3,5-dimethoxybenzene | HCID 69365590 | 94,1% |
Reaktionsschritte
To a solution of 3,5-dimethoxyphenol (6.73 g, 43.7 mmol) in anhydrous dimethylformamide (50 mL) were added imidazole (5.95 g, 87.4 mmol) and t-butylchlorodiphenylsilane (15.0 g, 54.6 mmol), and the mixture was stirred at 50° C. for 4 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate-hexane (1:2). The organic layer was washed with water, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel to yield 1-t-butyldiphenylsiloxy-3,5-dimethoxybenzene as a colorless crystalline powder (melting point: 95.5-96.5° C.) (16.14 g, yield: 94%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06706703B2 |
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| Quelldatensatz | uspto-grants-2004_03 |
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| ORD ID | ord-44d6565d2ae8422c8393a77b123d9947 |
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| Quellennotiz | uspto-grants-2004_03 |
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