Method for synthesizing liquid crystal medium
A technology of liquid crystal medium and synthesis method, applied in liquid crystal materials, chemical instruments and methods, etc., can solve the problems of low final yield and low comprehensive yield, etc.
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Embodiment 1-1
[0059] Example 1-1: Preparation of 4'-bromo-2'-ethyl-4-methoxy-[1,1'-biphenyl]-3-carbaldehyde
[0060] Add 3-formyl-4-methoxyphenylboronic acid (5.37g, 30mmol), 4-bromo-2-ethyliodobenzene (9.33g, 30mmol), potassium carbonate (8.28g, 60mmol) into a 250ml two-necked bottle ), toluene 60ml, ethanol 15ml, water 15ml, stirred at room temperature, and replaced nitrogen several times, then added tetrakis (triphenylphosphine) palladium (2.34g, 2.03mmol), stirred at room temperature for 20 minutes, then Heat to 90°C and react for 6 hours, TLC traces until the reactant disappears and the reaction is completed, add an equal amount of water to the reaction solution, extract with ethyl acetate, wash the organic phase with water, dry, concentrate under reduced pressure, and separate by column chromatography to obtain white Solid 6.50g, yield 68%. 1H-NMR (500 MHz, CDCl3) δ 10.51 (s, 1H), 7.75 (d, J = 2.4 Hz, 1H), 7.46 (dd, J = 8.5, 2.4 Hz, 1H), 7.43 (d, J = 2.0 Hz, 1H), 7.34 (dd, J = 8.1, ...
Embodiment 1-2
[0061] Example 1-2: Preparation of 4'-chloro-2'-ethyl-4-methoxy-[1,1'-biphenyl]-3-carbaldehyde
[0062] Add 4-chloro-2-ethylphenyl trifluoromethanesulfonate (8.66g, 30mmol), 4-bromo-2-ethyliodobenzene (9.33g, 30mmol), potassium carbonate ( 8.28g, 60mmol), tetrahydrofuran 90ml, stirred at room temperature, and replaced nitrogen several times, then added [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride (1.76g, 2.40 mmol), stirred at room temperature for 20 minutes, then heated to 110°C for 3 hours, after the reaction was completed, an equal amount of water was added to the reaction solution, extracted with ethyl acetate, the organic phase was washed with water, dried, concentrated under reduced pressure, and Separation by column chromatography yielded 5.27 g of a white solid with a yield of 64%. 1 H-NMR (500 MHz, CDCl3) δ 10.50 (s, 1H), 7.73 (d, J = 2.4 Hz, 1H), 7.42 (dd, J = 8.5, 2.4 Hz, 1H), 7.40 (d, J = 2.0 Hz, 1H), 7.32 (dd, J = 8.1, 1.9 Hz, 1H), 7.02 (d, J = 8.6...
Embodiment 2
[0063] Example 2: Preparation of 2'-ethyl-4-methoxy-4''-pentyl-[1,1':4',1''-terphenyl]-3-carbaldehyde
[0064] Method 1: Add 4'-bromo-2'-ethyl-4-methoxy-[1,1'-biphenyl]-3-carbaldehyde (3.19g, 10mmol) and 4-pentane to a 100ml two-necked bottle Phenylboronic acid (2.88g, 15mmol), potassium carbonate (2.76g, 20mmol), toluene 20ml, ethanol 5ml, water 5ml, stirred at room temperature, and replaced nitrogen several times, then added tetrakis (triphenylphosphine) palladium (0.81g, 0.70mmol), stirred at room temperature for 20 minutes. Then heated to 90°C for 6 hours. After the reaction was completed, an equivalent amount of water was added to the reaction solution, extracted with ethyl acetate, the organic phase was washed with water, dried, concentrated under reduced pressure, and separated by column chromatography to obtain 3.89 g of a white solid with a yield of 99%.
[0065] Method 2: Add 4'-chloro-2'-ethyl-4-methoxy-[1,1'-biphenyl]-3-carbaldehyde (2.75g, 10mmol) and 4-pentane ...
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