Liquid crystal compound and its preparation method and use
A liquid crystal compound and selected technology, applied in the field of liquid crystal materials, can solve the problems of TFT-LCD such as insufficient fast response, low viscosity, and insufficient charge retention rate
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Embodiment 1
[0083] Embodiment 1: intermediate Preparation of 4'-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]bicyclohexylcarbaldehyde (Compound 7)
[0084] 1) Synthesis of 2,3-difluoro-4-(2-fluoroethoxy)-bromobenzene (compound 2)
[0085]
[0086]Add 22mL of N,N-dimethylformamide into a 50mL reaction bottle, start stirring, add 5.2g of 2,3-difluoro-4-bromophenol (compound 1), after the solid is completely dissolved, add 10mL of water, 0.25g Tetrabutylammonium bromide, 4.0g anhydrous potassium carbonate. Heat up, control the temperature at 65-72°C, add 4.9g of 2-fluoroiodoethane dropwise, stir for 4 hours, add 10mL of toluene and 15mL of water, stir for 10 minutes, let stand to separate the liquid, and extract the water phase twice with 5mL×2 toluene (Stir for 2 minutes, let stand for 5 minutes), discard the water phase. All organic phases were combined and washed three times with 10 mL×3 water. The solvent was spin-dried and distilled under reduced pressure to obtain compound 2. Theor...
Embodiment 24
[0155] Synthesis of Example 24-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]-4'-vinyl-bicyclohexane (compound 8)
[0156]
[0157] Add 41.8g of methyl iodide phosphonium salt and 200mL of tetrahydrofuran into a 1L three-necked flask, cool down to minus 10°C, add 14.3g of potassium tert-butoxide, and react for 1 hour. Temperature controlled dropwise addition of 50mL tetrahydrofuran and 25.4g 4'-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]bicyclohexylformaldehyde (compound 7) mixed solution, natural heating reaction, stirring overnight , add 200mL of water, 100mL of ethyl acetate, stir, let stand to separate the liquid, concentrate the solvent, add 3 times the theoretical amount of petroleum ether, heat to 75 ° C, pass through a silica gel alumina heat column, concentrate the solvent to obtain 24.8g, add 2 times the theoretical amount of petroleum ether Hydro-ethanol recrystallization three times. Compound 8 was obtained, theoretical yield: 25.2 g, actual yield: 19.6 g, yield: 78.0%....
Embodiment 34
[0168] Example 3 Synthesis of 4'-(but-3-enyl)-4-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]bicyclohexane (compound 11)
[0169] 1) Synthesis of {4'-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]-bicyclohexyl}methanol (compound 9)
[0170]
[0171] A solution consisting of 77g of 4'-[2,3-difluoro-4-(2-fluoroethoxy)-phenyl]bicyclohexylformaldehyde (compound 7) and 200L of tetrahydrofuran in a 1L three-necked flask, temperature controlled at 0-10°C, 10.0 g of solid potassium borohydride was added in portions, and the addition was completed in about 30 minutes. Keep warm at 40-50°C for 3 hours. Control the temperature below 20°C, slowly add a solution consisting of 50mL of hydrochloric acid and 100mL of water dropwise, add 100mL of water and 100mL of dichloromethane into the reaction kettle, heat slightly to about 35°C, let stand to separate the liquid, and separate the lower product layer, The upper aqueous phase was extracted with 100 mL of dichloromethane, and the organic phases ...
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