(三乙氧基硅基)环己烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 60 ml of dry diethyl ether and 14.0 gram (0.067 mole) of tetraethoxysilane were charged in a 250 ml flask equipped with a reflux condenser and a stirring apparatus in an atmosphere of nitrogen and above prepared solution of cyclohexyl magnesium chloride was slowly added while keeping the internal temperature below 10° C. After completion of addition stirring was carried out at room temperature for 6 hours and at reflux temperature for 2 hours. To the resulting reaction mass 10-20 ml of saturated aqueous ammonium chloride solution was added drop wise to dissolve magnesium salt. The organic layer was separated from the aqueous layer, dried and evaporated to give crude cyclohexyltriethoxysilane. This crude was purified by fractional distillation under reduced pressure, yielding 14.2 gram of pure cyclohexyltriethoxysilane (86% of the theoretical maximum yield based on the amount of tetraethoxysilane). equipped with a reflux condenser was slowly added the internal temperature below 10° C After completion of addition at reflux temperature for 2 hours was added drop wise The organic layer was separated from the aqueous layer dried evaporated to give crude cyclohexyltriethoxysilane This crude was purified by fractional distillation under reduced pressure