Reaktion #12072

Reaktionsgleichung

CF2═CFCl

sec-BuLi

Si(OEt)4

→

CF2═CFSi(OEt)3

Lösungsmittel

Et2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATION200 ml of freshly distilled dry Et2O
2. 2
   workup.ADDITIONis added to a 500 ml vessel (under an argon atmosphere)
3. 3
   Sonstigeis kept below −60° C.
4. 4
   workup.STIRRINGThe solution is stirred for over night
5. 5
   Temperaturto warm up to room temperature
6. 6
   SonstigeFormed red solution
7. 7
   Filtrationis filtered
8. 8
   Sonstigeevaporated to dryness

Vorschrift

200 ml of freshly distilled dry Et2O is added to a 500 ml vessel (under an argon atmosphere). The vessel is cooled down to −80° C. and 15 g (0.129 mol) of CF2═CFCl gas is bubbled to Et2O. 100 ml (0.13 mol) of sec-BuLi is added dropwise during three hours. The temperature of the solution is kept below −60° C. all the time. The solution is stirred for 15 minutes and 29 ml (27.08 g, 0.130 mol) of Si(OEt)4 is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed red solution is filtered and evaporated to dryness to result crude trifluorovinyltriethoxysilane, CF2═CFSi(OEt)3.

Quelle