Liquid crystal compound with negative dielectric anisotropy as well as preparation method and application thereof
A liquid crystal compound, anisotropic technology, applied in chemical instruments and methods, liquid crystal materials, etc., can solve problems such as long response time, achieve high-definition bright spots, good stability and UV resistance, large dielectric anisotropy absolute value effect
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[0031] Example 1
[0032] A compound The preparation method, wherein the preparation route is as follows:
[0033]
[0034] The specific synthesis method is:
[0035] 1. 57.9g 2,3-difluorobromobenzene is made into Grignard reagent with THF, cooled to -20℃, 19.1g acetaldehyde is added dropwise to the Grignard reagent, the temperature is controlled at -20℃, and the temperature rises to room temperature naturally , Stir for 2h, spin dry, add aqueous ammonium chloride solution, extract with EA; wash the EA phase twice with saturated brine, and dry; add 300ml THF, 30ml TFA, stir for 12h, spin dry to obtain 40.6g of the above compound 1.
[0036] 2. 40.6g of compound 1, 0.3g of palladium-carbon in 300ml of ethanol, hydrogenation with hydrogen at atmospheric pressure for 5h, filtered, spin-dried to obtain 41.1g of the above compound 2.
[0037] 3. 41.1g of compound 2 was dissolved in 200ml of THF, cooled to -78°C, 119ml of butyllithium was dripped at -70°C, heated to -60°C, stirred for 1h; c...
Example Embodiment
[0044] Example 2
[0045] A compound The preparation method, wherein the preparation route is as follows:
[0046]
[0047] The specific synthesis method is:
[0048] 1. Synthesis of compound 3, the synthesis method is the same as the synthesis method of compound 3 in Example 1.
[0049] 2. 41g compound 3, 38.2g 1,2-difluorobromobenzene, 60g potassium phosphate, 0.5g tetrakistriphenylphosphonium palladium, 300ml toluene, stir 8h at 90℃ under nitrogen protection; cool, concentrate, add EA, use Washed with saturated brine for 3 times, dried with anhydrous sodium sulfate, filtered, and spin-dried to obtain 48.3 g of compound 9.
[0050] 3. 48.3g of compound 9 was dissolved in 200ml of THF, cooled to -78°C, 84ml of butyllithium was dropped at -70°C, heated to -40°C, and stirred for 1h. Cool to -78°C, drop 48 g of tributyl borate into it, warm to room temperature naturally, and stir for 6 hours. Add 200 ml of water containing 40 ml of concentrated hydrochloric acid, stir for 0.5 h, and s...
Example Embodiment
[0069] Example 4
[0070] A compound The preparation method, wherein the preparation route is as follows:
[0071]
[0072] The specific synthesis method is:
[0073] 1. Synthesize compound 13, and the synthetic method is the same as that of compound 13 in Example 2.
[0074] 2. 57g compound 13, 17g p-propylphenylboronic acid, 40g potassium phosphate, 0.5g tetrakistriphenylphosphonium palladium, 200ml toluene, stirring at 90℃ for 8h under nitrogen protection; cooling, concentration, adding EA, washing with saturated brine 3 times, dried with anhydrous sodium sulfate, filtered, and spin-dried to obtain 54.7 g of compound 22.
[0075] 3. 54.7g of compound 22, 360ml of ethanol, and 0.1g of TBAF were stirred for 12 hours; 43g of compound 23 was obtained by rotary drying.
[0076] 4. 43g of compound 23, 8.7g of manganese dioxide, 150ml of THF, stirred at room temperature for 12h. Filter and spin dry to obtain 42 g of compound 24.
[0077] 5. 42g of compound 24, 7.1g of hydroxylamine hydroch...
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