Novel liquid crystal compound-3-(4-n-dekaoxylbenzyl)acrylic acid-2-fluo-4-hydroxybenzenenitrile ester and its preparation method
A technology of n-decyloxyphenyl and liquid crystal compounds, which is applied in the field of substituted phenyl acrylate organic liquid crystal compounds and its preparation, can solve the problems of low viscosity and low working voltage, achieve high clearing point, wide liquid crystal range, chemical stable effect
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Embodiment 1
[0015] 1) Dissolve 0.01mol of 3-(4-hydroxyphenyl)acrylic acid and 0.02mol of potassium hydroxide in 40ml of 95% (volume fraction) ethanol, then add 0.03mol of brominated n-decane dropwise at a rate of about 1ml / min , Reflux reaction for 24h, then add 14ml of 70% (volume fraction) ethanol solution of 0.02mol potassium hydroxide, and continue to reflux for 2h. Add 100ml of water, 20ml of concentrated hydrochloric acid, heat for 15min, cool and filter, wash with distilled water, dry, and recrystallize with 95% (volume fraction) ethanol to obtain 3-(4-n-decyloxyphenyl)acrylic acid, which is white Flaky crystals, yield 53%.
[0016] 2) Add 0.01mol of 3-(4-n-decyloxyphenyl)acrylic acid and 20ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.01mol of DCC (N,N-dicyclohexylcarbodi imine), after turbidity occurs, dissolve 0.01mol 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] in 20ml of anhydrous...
Embodiment 2
[0018] 1) Dissolve 0.02mol of 3-(4-hydroxyphenyl)acrylic acid and 0.05mol of potassium hydroxide in 100ml of 95% (volume fraction) ethanol, then add 0.05mol of iodo-n-decane dropwise at a rate of about 1ml / min , Reflux reaction for 48h. Then add 35 ml of 0.04 mol potassium hydroxide in 70% (volume fraction) ethanol solution, and continue to reflux for 2 h. Add 100ml of water and 40ml of concentrated hydrochloric acid, mix well, heat for 20min, cool and filter, wash with distilled water, dry, and recrystallize with 95% (volume fraction) ethanol to obtain 3-(4-n-decyloxyphenyl)acrylic acid , as white flaky crystals, with a yield of 49%.
[0019] 2) Add 0.015mol of 3-(4-n-decyloxyphenyl)acrylic acid and 50ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.015mol of DCC (N,N-dicyclohexylcarbodi imine), after turbidity appeared, 0.015mol 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] were co...
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