反应详情

温度

90 °C

Under a nitrogen atmosphere a 1-liter, 3-necked flask equipped with a heating mantle, magnetic stirrer, pot thermometer, addition funnel and condenser was charged with 276.8 g of a mixture of approximately 46% (dichlorosilylmethyl)trichlorosilane and 54% bis(trichlorosilyl)methane [molar ratio 1:1]. The mixture was heated to 90° C. and 10 g of decene were added to the mixture via addition funnel, followed by 0.5 ml of 5% hexachloroplatinic acid in tetrahydrofuran. An immediate exotherm was observed and the reaction mixture changed from clear to dark brown. An additional 173 g of decene were added at an appropriate rate to maintain the temperature between 90 and 110° C. Upon completion of the addition, an additional 0.25 ml of 5% hexachloroplatinic acid solution was added and the mixture was stirred at 100° C. for 45 minutes. GC analysis of the mixture indicated the presence of some unreacted pentachlorodisilapropane. An additional 10 g of decene were added and the reaction mixture was stirred an additional 45 minutes at 100° C. Distillation provided 242 g (59%) of the title compound, bp 126° C./0.1 mm Hg, density @ 20° C. 1.180.

1. customUnder a nitrogen atmosphere a 1-liter, 3-necked flask equipped with a heating mantle, magnetic stirrer
2. additionpot thermometer, addition funnel and condenser
3. temperatureto maintain the temperature between 90 and 110° C
4. additionUpon completion of the addition
5. stirringthe reaction mixture was stirred an additional 45 minutes at 100° C
6. distillationDistillation