3,3,3-Trifluoropropyl-trimethoxysilane → 3,3,3-Trifluoropropyl(cyclopentyl)dimethoxysilane

HRID 1029379

Reaktionsgleichung

Reaktionsgleichung von HRID 1029379
[CH:1]1([Mg]Cl)[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:8][C:9]([F:20])([F:19])[CH2:10][CH2:11][Si:12](OC)([O:15][CH3:16])[O:13][CH3:14].[SiH4].CCCCCC>C(OCC)C.CCCCCC>[F:20][C:9]([F:8])([F:19])[CH2:10][CH2:11][Si:12]([CH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1)([O:13][CH3:14])[O:15][CH3:16]

Komponenten

6

Edukt 3

HCID 679333,3,3-Trifluoropropyl-trimethoxysilaneHCID 131717238Silane hexaneHCID 178478989HCID 178478989, Verbindung

Produkt 1

HCID 199000453,3,3-Trifluoropropyl(cyclopentyl)dimethoxysilane

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittel2×HCID 8058HexaneLösungsmittel

Versuchsvorschrift

Under nitrogen, a 500 ml Schlenk flask was cooled to room temperature, charged with 150 ml of diethyl ether and cyclopentylmagnesium chloride (0.055 mol, 27.7 ml) and warmed slightly to 30° C. A 100 ml Schlenk flask was purged with nitrogen and charged with 75 ml hexane and 3,3,3-trifluoropropyltrimethoxy silane (10 ml, 0.0504 mol). The silane/hexane solution was added dropwise via cannula to the Grignard/diethyl ether mixture producing a white cloudy mixture. After addition (1.25 hrs.), the Grignard containing flask was rinsed once with 25 ml of hexane. The reaction mixture was stirred at room temperature for one hour.

Aufarbeitung

  1. temperaturewarmed slightly to 30° C
  2. customA 100 ml Schlenk flask was purged with nitrogen
  3. customproducing a white cloudy mixture
  4. additionAfter addition (1.25 hrs.)
  5. additionthe Grignard containing flask
  6. washwas rinsed once with 25 ml of hexane

Quellen und Nachweise

ORD-Eintrag
ord-dc2a1dd5867444178c2fa5cf1148e5a1
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05102842

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