Reaktion #1061568

Reaktionsgleichung

tetrahydrofuran

t-butyl chloride

magnesium

diphenyldichlorosilane

→

tert-butyldiphenylchlorosilane

Ausbeute 75.0%

Lösungsmittel

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a reflux condenser, addition funnel
2. 2
   SonstigeAfter drying under a nitrogen atmosphere
3. 3
   workup.STIRRINGwith stirring
4. 4
   workup.STIRRINGwhile stirring
5. 5
   Sonstigerose to 50 degrees Centigrade
6. 6
   TemperaturAfter heating
7. 7
   workup.STIRRINGstirring
8. 8
   Temperaturunder reflux for 5 hours
9. 9
   workup.DISTILLATIONcontinuing with distillation in vacuo

Vorschrift

12.2 g (0.5 mol) magnesium was introduced into a 500 mL four-neck flask equipped with a reflux condenser, addition funnel, thermometer, and stirring rod. After drying under a nitrogen atmosphere, the tert-butyl Grignard reagent was prepared by the addition of 250 mL tetrahydrofuran and 46.3 g (0.5 mol) t-butyl chloride with stirring. To this was added 0.45 g (0.005 mol) copper cyanide at room temperature, and 126.6 g (0.5 mol) diphenyldichlorosilane was then dripped in while stirring. The system temperature rose to 50 degrees Centigrade. After heating and stirring under reflux for 5 hours, the addition of 100 mL hexane, filtration, distillation of the solvent, and continuing with distillation in vacuo gave 103 g (yield =75%) tert-butyldiphenylchlorosilane.

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