Silane → Octanal, pentadecafluoro-

HRID 1721697

Reaktionsgleichung

Reaktionsgleichung von HRID 1721697
C([SiH](C(C)C)C(C)C)(C)C.[F:11][C:12]([F:35])([C:16]([F:34])([F:33])[C:17]([F:32])([F:31])[C:18]([F:30])([F:29])[C:19]([F:28])([F:27])[C:20]([F:26])([F:25])[C:21]([F:24])([F:23])[F:22])[C:13](Cl)=[O:14].[SiH4]>[Pd]>[C:12]([CH:13]=[O:14])([C:16]([C:17]([C:18]([C:19]([C:20]([C:21]([F:22])([F:23])[F:24])([F:25])[F:26])([F:28])[F:27])([F:30])[F:29])([F:32])[F:31])([F:34])[F:33])([F:35])[F:11]

Komponenten

5

Edukt 3

HCID 23953SilaneHCID 78978Perfluorooctanoyl chlorideHCID 138754Silane, tris(1-methylethyl)-

Produkt 1

HCID 533723Octanal, pentadecafluoro-Ausbeute 89,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23938PalladiumKatalysator

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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 aidehyde/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.

Aufarbeitung

  1. temperatureto warm to room temperature
  2. customwas then controlled at 25°-27° C. during the exothermic reaction
  3. waitwas continued for 1 hr
  4. customVacuum transfer gave liquid which
  5. temperaturewas chilled at -25° C
  6. temperaturechilled at -25° C.
  7. customseparated again

Quellen und Nachweise

ORD-Eintrag
ord-02a1b25da8da410cb751185fae76f431
Quelldatensatz
uspto-grants-1996_04
Patentnummer
US05512652

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