Reaktion #1786691

Reaktionsgleichung

fluorine

dimethoxyethane

diphenyldichlorosilane

butyllithium

→

2a

Ausbeute 66.0%

Chlorodiphenyl-1-(9-fluorenyl)silane

Ausbeute 66.0%

Lösungsmittel

toluene

heptane

heptane

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to −30° C.
2. 2
   workup.ADDITIONadded to a solution
3. 3
   workup.STIRRINGAfter stirring for 1.5 hours at room temperature
4. 4
   Temperaturthe suspension was heated to 60° C.
5. 5
   Filtrationthe lithium chloride was filtered off
6. 6
   SonstigeAfter removal of the solvent
7. 7
   Sonstigethe solid which precipitated
8. 8
   Filtrationfiltered off
9. 9
   Waschenwashed with heptane until virtually colorless and
10. 10
    Sonstigedried under reduced pressure

Vorschrift

80 g (0.48 mol) of fluorine and 160 ml of toluene/12.8 ml (0.12 mol) of dimethoxyethane (DME) were placed in a reaction vessel and admixed with 182 ml (0.48 mo) of a 20% strength solution of butyllithium in toluene. The suspension was stirred for another 2 hours at 50° C. The suspension was diluted with 400 ml of heptane, cooled to −30° C. and added to a solution, cooled to −30° C., of 182 g (0.72 mol) of diphenyldichlorosilane in 400 ml of heptane. After stirring for 1.5 hours at room temperature, the suspension was heated to 60° C. and the lithium chloride was filtered off. After removal of the solvent, the solid which precipitated was suspended in heptane, filtered off, washed with heptane until virtually colorless and dried under reduced pressure. 123 g (66%) of 2a were obtained.

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