Liquid crystal aligning agent and liquid crystal display element
A technology of liquid crystal aligning agent and carboxylic acid, which is applied in liquid crystal materials, chemical instruments and methods, instruments, etc., can solve the problems of more and more severe harshness, and achieve good storage stability, less reduction in voltage retention, and liquid crystals. Excellent orientation effect
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Synthetic example 1
[0375] In a reaction vessel with a stirrer, thermometer, dropping funnel and reflux condenser, add 100.0 g of 2-(3,4-epoxycyclohexyl) ethyl trimethoxysilane, 500 g of methyl isobutyl ketone and 10.0 g of triethylamine, mixed at room temperature. Next, after adding 100 g of deionized water dropwise over 30 minutes from the dropping funnel, it was reacted at 80° C. for 6 hours while mixing under reflux. After the reaction, the organic layer was taken out, washed with 0.2% by weight of ammonium nitrate aqueous solution until the washed water was neutral, and the solvent and water were distilled off under reduced pressure to obtain polyorganosiloxane EPS-1, which was viscous Transparent liquid.
[0376] The polyorganosiloxane EPS-1 is carried out 1 In the H-NMR analysis, a peak based on the oxiranyl group was obtained at a chemical shift (δ)=3.2ppm near the theoretical intensity, and it was confirmed that no side reaction occurred in the epoxy group during the reaction.
[0377...
Synthetic example 2
[0382] 1.80 g of monomethyl terephthalate, 3.27 g of di-tert-butyl dicarbonate, and 25 ml of THF were mixed and stirred at room temperature for 10 minutes. After adding 0.37 g of 4-dimethylaminopyridine, the reaction was stirred at 25° C. for 6 hours. After mixing with ethyl acetate, it was washed with saturated aqueous sodium bicarbonate and distilled water. Concentration and drying yielded 1.54 g of the target intermediate. 1.16g of the above intermediate, 0.42g of lithium hydroxide monohydrate, 6ml of methanol, and 2ml of distilled water were mixed, and stirred and reacted at 25°C for 1 hour. After mixing with 50 ml of ethyl acetate, it was washed with dilute hydrochloric acid and distilled water, and concentrated. The resulting powder was mixed with chloroform, and the insoluble components were removed by filtration. The filtrate was concentrated and dried to obtain 0.80 g of compound b (B-1-1) as a white powder.
Synthetic example 3
[0384] According to the following routes, 45 g of compounds represented by compound b (B-1-2) were obtained respectively.
[0385]
[0386] 5.0 g of (1,1-dimethylethyl)methyl 1,3-benzoate, 16.35 g of di-tert-butyl dicarbonate, and 50 ml of THF were mixed, and stirred at room temperature for 10 minutes. After adding 1.85 g of 4-dimethylaminopyridine, the reaction was stirred at 25° C. for 6 hours. After mixing with ethyl acetate, it was washed with saturated aqueous sodium bicarbonate and distilled water. Concentration and drying yielded 7.70 g of the target intermediate. 5.80 g of the above intermediate, 2.10 g of lithium hydroxide monohydrate, 20 ml of methanol, and 4 ml of distilled water were mixed, and stirred and reacted at 25° C. for 1 hour.
[0387] After mixing with 50 ml of ethyl acetate, it was washed with dilute hydrochloric acid and distilled water, and concentrated. The resulting powder was mixed with chloroform, and the insoluble components were removed by ...
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