Synthesis
In a 1000 mL reaction flask, Put in xylene 230g, Sodium metal 47g, TDA-1 0.37g, Warm up to 100110°C, Insulation 0.5h, and Turn on stirring. After stirring for 1 hour, all the sodium was made into sodium sand, and a Sodium sand mixture was formed. After 73.5 g of p-dichlorobenzene and 100 g of xylene were mixed and dissolved, Then add 96.5g of dimethylchlorosilane Formed a mixture; the mixture was added to a constant-pressure funnel. The liquid droplets in the constant pressure funnel are added to the sodium sand mixture. Dropping about 5h to complete, the reaction was completed by keeping it at 100-110°C for 2 hours. After the reaction, Cool the reaction system to 5-15°C. Then, add 280 mL of water from the constant pressure funnel. Stirring 1h, Stand for 1h, Then separate the lower brine phase, The upper organic phase is taken as the crude 1,4-bis (dimethylsilyl) benzene. The upper organic phase is entered into the distillation flask, and the temperature in the control bottle is below 120°C. Vacuum distillation,92 g of 1,4-Bis(dimethylsilyl)benzene was obtained; the yield is 95%.
