Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Silane | HCID 23953 | — |
| Edukt | Perfluorooctanoyl chloride | HCID 78978 | — |
| Edukt | Silane, tris(1-methylethyl)- | HCID 138754 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Produkt | Octanal, pentadecafluoro- | HCID 533723 | 89,4% |
Reaktionsschritte
Catalyst 10% Pd/C(200 mg) was placed in a 3-necked round bottom flask and cooled at 0° C. Triisopropylsilane (3.32 g, 21 mmol) was added, followed by perflurooctanoyl chloride (7.9 g, 18.2 mmol). The mixture was allowed to warm to room temperature and was then controlled at 25°-27° C. during the exothermic reaction. After 3 hr, GC analysis showed aldehyde/acid chloride ratio=94/6. Another 0.26 mL of silane was added and stirring was continued for 1 hr. Vacuum transfer gave liquid which was chilled at -25° C. The resulting solid was shaken with petroleum ether, chilled at -25° C., and separated again. In this way, 6.48 g of product was obtained, mp ca. -5° C. NMR spectra were as described in Example 1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05414140 |
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| Quelldatensatz | uspto-grants-1995_05 |
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| ORD ID | ord-d1b41ca9f9ea4361a4a5dbb77a26cd47 |
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| Quellennotiz | uspto-grants-1995_05 |
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