A pendant ethyl fluorine-containing triphenyldiyne liquid crystal compound and its preparation method, liquid crystal composition and application
A liquid crystal compound and liquid crystal composition technology, applied in chemical instruments and methods, liquid crystal materials, etc., can solve the problems of large dielectric loss of liquid crystal materials, increase of microwave phase shift, and small Δn value, etc., to achieve dielectric loss Low, excellent dielectric properties, low melting point effect
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[0058] In one embodiment of the preparation method of the liquid crystal compound provided by the present invention, in combination with the above synthetic route, R in the structural formula (I) 1 for-C 3 h 7 , X 1 for-F,X 2 、X 3 and x 4 for H, Z for C 2 h 11 As an example for illustration, the preparation method of the liquid crystal compound includes the following steps:
[0059] Step S10: Mix and stir o-ethylaniline, iodine, calcium carbonate powder and water for 50-70 minutes, then raise the temperature to 60-80°C for 0.5-2 hours, cool the reaction solution to room temperature after the reaction, and then use dichloro After methane dissolves the reaction solution, the organic layer is separated, and the obtained organic layer is purified to obtain a purple solid, which is intermediate a;
Embodiment 1
[0122] The synthesis of embodiment 1 liquid crystal compound 3GTPI (2) TP5, structural formula is:
[0123]
[0124] Its synthetic route is as follows:
[0125]
[0126] The preparation process is:
[0127] (1) Add 8.3 g of redistilled 2-ethylaniline (0.066 mol), 16.8 g of iodine (0.066 mol), and 8.3 g of CaCO in a three-neck flask (250 mL) equipped with a condenser tube and a thermometer. 3 Powder (0.083mol) and 80mL deionized water were stirred at room temperature for 1 h, and then the temperature was raised to 70°C for 2 h. During the reaction, TLC was used to spot the plate (the developer was selected from ethyl acetate and petroleum ether with a volume ratio of 1:10) mixed solvent) to track and detect the reaction process until the reaction is complete, and the reaction solution is mixed with CH 2 Cl 2 Suction filtration is carried out after dissolving, then static stratification and separate organic layer, organic layer is washed with anhydrous Na 2 SO 4 After...
Embodiment 2
[0137] The synthesis of embodiment 2 liquid crystal compound 3UTPI (2) TP5, structural formula is:
[0138]
[0139] Its synthetic route is as follows:
[0140]
[0141] The preparation process is:
[0142] (1) to (3): Same as Example 1.
[0143](4) Add intermediate c (compound 5PTP(2) Br, 0.026mol, 9g), 1-propyl-3,5-difluorobenzene-4-acetylene (0.026mol , 4.7g), bis(triphenylphosphine) palladium chloride (1mol%, 0.07g), triphenylphosphine (3mol%, 0.07g), cuprous iodide (2mol%, 0.04g), then add 100mL triethylamine, then heated up to the solvent reflux reaction for 5h under the condition of nitrogen protection. During the reaction, TLC spot plate (petroleum ether was used as developing agent) was used to track the progress of the reaction; after the reaction was completed, the reaction solution was suction filtered and the filtrate was collected. , remove the solvent in the filtrate by distillation under reduced pressure; pour 100mL ethyl acetate into the filtrate agai...
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Abstract
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