A kind of liquid crystal compound and its preparation method and application
A liquid crystal compound and compound technology, applied in the preparation of organic compounds, chemical instruments and methods, liquid crystal materials, etc., can solve the problems of insufficient charge retention, low dielectric anisotropy, low viscosity, etc.
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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 N,N-dimethylformamide into a 50mL reaction bottle, start stirring, add 5.2g 2,3-difluoro-4-bromophenol (compound 1), after the solid is completely dissolved, add 10mL water, 0.25g Butylammonium bromide, 4.0 g 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. Theoretical yield:...
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 dropwise a solution consisting of 50mL hydrochloric acid and 100mL water, add 100mL water and 100mL dichloromethane into the reaction kettle, heat slightly to about 35°C, let stand to separate the liquid, separate the lower product layer, the upper layer The aqueous phase was extracted with 100 mL of dichloromethane, and the organic phases were c...
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