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ChemicalBook CAS DataBase List 1,4-Bis(dimethylsilyl)benzene
2488-01-9

1,4-Bis(dimethylsilyl)benzene synthesis

2synthesis methods
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%.
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Yield:2488-01-9 95%

Reaction Conditions:

with Tris(3,6-dioxaheptyl)amine;sodium in 5,5-dimethyl-1,3-cyclohexadiene at 100 - 110; for 7 h;Concentration;

Steps:

2 Example 2
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,Turn on stirringAfter stirring for 1 hour, all the sodium was made into sodium sand,Sodium sand mixture is formed.After 73.5 g of p-dichlorobenzene and 100 g of xylene were mixed and dissolved,Then add 96.5g dimethylchlorosilane,Form 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,Then the reaction was completed by keeping 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 into the distillation flask,The temperature in the control bottle is below 120°C.Vacuum vacuum distillation,92 g of 1,4-bis (dimethylsilyl) benzene was obtained,The yield is 95%.Purity greater than 99%.

References:

Yangzhou San You Synthetic Chemical Co., Ltd.;Li Huining;Zhang Yang;Li Mingcheng;Zhang Caishan CN107698616, 2018, A Location in patent:Paragraph 0012-0021

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