Liquid crystal compound and preparation method thereof as well as liquid crystal mixture containing liquid crystal compound and application of liquid crystal mixture
A technology of liquid crystal compounds and compounds, which is applied in the field of liquid crystal mixtures, liquid crystal compounds, and their preparation, can solve the problems of insufficient response speed of liquid crystal materials, and achieve the effects of meeting various performance requirements, improving mixing and mutual solubility, and reducing response time
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[0027] In another typical embodiment of the present application, a preparation method of the above-mentioned liquid crystal compound is provided, the preparation method comprising: compound A, compound B, ethanol, potassium carbonate, Pd( PPh 3 ) 4 , toluene and water are mixed to form a first reaction system; the first reaction system is stirred at 80-85°C for 8-10 hours to obtain a liquid crystal compound, wherein compound A has a structural formula A, compound B has a structural formula B, and the structural formula A is : Structural formula B is: R 3 and R 4 Different, one of them is B(OH) 2 , and the other is a halogen. The above preparation method is simple to operate, and the purity of the liquid crystal compound in the product is relatively high, and the stirring method of the first reaction system is preferably reflux stirring.
[0028] Compound A and Compound B in the above scheme can be synthesized by using various synthetic methods in the prior art. Accord...
Embodiment 1
[0071] (PPFP2Cp) synthesis, the synthetic route is as follows:
[0072]
[0073] The specific process steps are as follows:
[0074] (1), 50.4g anhydrous magnesium tablet, 50ml anhydrous tetrahydrofuran and several grains of iodine are placed in a clean and dry 3000ml four-necked flask, heated under nitrogen protection to initiate the reaction, then 374g compound 1 and 2000ml anhydrous tetrahydrofuran The mixture was slowly added dropwise to the above reaction system, and the temperature was controlled to ~65°C. After the drop was completed, the mixture was heated under reflux and stirred for 2 hours to obtain compound 2, which was cooled to room temperature for later use; the above compound 2 was slowly added dropwise to the 2 , 350g of m-fluorobromobenzene and 500ml of anhydrous tetrahydrofuran in a 5000ml three-necked flask, control the temperature to 0°C, continue stirring for 1 hour after dropping, then raise the temperature to 60-65°C for 2.5 hours to obtain the cru...
Embodiment 2
[0078] compound (PPFPCCp5) synthesis, the synthetic route is as follows:
[0079]
[0080] (1), under nitrogen protection at 80-85°C, put 240g compound 6, 140g m-fluorophenylboronic acid, 138g potassium carbonate, 5.5gPd(PPh3)4, 300ml toluene and 370ml water in a 2000ml four-necked flask, reflux, After stirring and reacting for 8-10 hours, wash with water, let stand to separate layers, collect the toluene phase in the upper layer, and distill the toluene off under reduced pressure. After distillation, the product was crystallized to obtain 230 g of compound 7 with a yield of 91%.
[0081] (2) Slowly add 200ml of n-butyllithium solution dropwise into a 2000ml four-necked flask containing 127g of compound 7, 85g of potassium tert-butoxide and 600ml of tetrahydrofuran through a constant pressure funnel, and control the reaction temperature at -70~-85°C , after the dropwise addition, heat preservation reaction for 1 hour; then slowly drop 78g of anhydrous tetrahydrofuran solu...
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