Tetraethoxysilane → Bis(pentafluorophenyl)diethoxysilane

HRID 11977

Reaktionsgleichung

Br[C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12].[Mg].C(O[Si:17]([O:24][CH2:25][CH3:26])([O:21][CH2:22][CH3:23])OCC)C>CCOCC>[F:8][C:7]1[C:2]([Si:17]([C:2]2[C:3]([F:12])=[C:4]([F:11])[C:5]([F:10])=[C:6]([F:9])[C:7]=2[F:8])([O:21][CH2:22][CH3:23])[O:24][CH2:25][CH3:26])=[C:3]([F:12])[C:4]([F:11])=[C:5]([F:10])[C:6]=1[F:9]

Komponenten

Reaktionsbedingungen

Temperatur: 35 °C

Versuchsvorschrift

265.2 mL (1.95 mol, 525.353 g) bromopentafluorobenzene, 52.11 g (2.144 mol) magnesium powder and 216 mL (0.975 mol, 203.025 g) tetraethoxysilane are mixed together at room temperature and diethylether is added dropwise to the vigorously stirred solution until an exothermic reaction is observed (˜240 ML). The solution is stirred for 30 minutes after which additional 90 mL of Et2O is carefully added. After stirring at 35° C. for 16 h the mixture is cooled to room temperature and diethylether evaporated. An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts. Solution is filtrated and evaporated to dryness. The residue is fractionally distilled under reduced pressure to yield di(pentafluorophenyl)diethoxysilane.

Aufarbeitung

additionis carefully added
temperatureis cooled to room temperature
customdiethylether evaporated
additionAn excess of n-heptane (˜600 mL) is added
customto precipitate the magnesium salts
filtrationSolution is filtrated
customevaporated to dryness
distillationThe residue is fractionally distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-a93a27bfb7fd4c638aa74d18829c69e1
Quelldatensatz: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07098346B2

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