Liquid crystal compound containing 4,6-dimethyl-1,3-dioxane ring, preparation method and applications thereof
A technology of liquid crystal compounds and dioxane, applied in chemical instruments and methods, liquid crystal materials, organic chemistry, etc., can solve the problems of insufficient voltage, insufficient response of TFT-LCD, and insufficient charge retention rate
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Embodiment 1
[0071]
[0072] The synthetic route for preparing compound LC-01 is as follows:
[0073]
[0074] (1) Step 1-1: Synthesis of compound 3
[0075] Add 0.3L toluene, 18.5g p-bromobenzaldehyde (compound 2, 0.1mol), 14.6g 2-propyl-1,3-dimethylpropanediol (compound 1, 0.1mol), 1.0g p-toluene to a 500mL three-necked flask Sulfonic acid, start stirring, and reflux for 6 hours. Post-processing: Add 100ml of water, separate the liquids, add 30g of anhydrous sodium sulfate to the organic phase and dry for 1 hour, then spin the solvent, add 200mL of petroleum ether, pass through a 50g silica gel column, and flush the column with 3 times the column height. The solvent was spin-dried to obtain 67 g of crude product, which was added with 2 times of ethanol, and then refrigerated (-30° C.) overnight for suction filtration. The product is a white solid with a gas phase purity (GC) of 99.0%, a theoretical yield of 36.4 g, an actual yield of 29.1 g, and a yield of 80%.
[0076] (2) Step...
Embodiment 2
[0083]
[0084] The synthetic route for preparing compound LC-02 is as follows:
[0085]
[0086] Add 40mL of absolute ethanol, 100mL of toluene and 100mL of water into a 500mL three-necked flask, start stirring, and add 35.4g of compound 4 (0.1mol), 31.3g of compound 3 (0.1mol) and 21.2g of anhydrous sodium carbonate (0.2mol). The nitrogen gas was substituted three times, and 0.40 g of tetrakis(triphenylphosphine)palladium was added. When heating to the liquid phase at 60°C, slowly heat to reflux and react at reflux for 8 hours. After the reflux was completed, 60 mL of water was added to the three-neck flask, stirred for 10 minutes, left to separate the liquids, and the organic phase was washed twice with 100 mL×2 water. Add 3 times of petroleum ether and heat to dissolve, and perform column chromatography. The solvent was spin-dried and recrystallized three times by freezing with 4 times ethanol, and suction filtered and air-dried to obtain a white solid LC-02 (compo...
Embodiment 3
[0092]
[0093] The synthetic route for preparing compound LC-03 is as follows:
[0094]
[0095] Add 0.4L of toluene, 32.6g of compound 6 (0.1mol), 14.6g of 2-propyl-1,3-dimethylpropanediol (compound 1, 0.1mol), 1.6g of p-toluenesulfonic acid into a 1000mL three-necked flask, and start stirring , reflux reaction for 6 hours. Post-processing: Add 100ml of water, separate the liquids, add 38g of anhydrous sodium sulfate to the organic phase and dry for 1 hour, then spin the solvent, add 300mL of petroleum ether, pass through a 60g silica gel column, and flush the column with 3 times the column height. Spin to dry the solvent, add 2 times of ethanol, refrigerate (-30°C) overnight, filter and dry to obtain white solid LC-03 (compound 7), gas phase purity (GC) 99.0%, theoretical yield 42.4g, actual yield 33.9g , yield 80%. Gas phase purity (GC) 99.9%.
[0096] Fragmentation by mass spectrometry: 424 (molecular ion peak).
[0097] 1 H-NMR (300MHz, CDCl 3 ):0.90-1.70(m,1...
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