Novel LCD compound p-n-hexyloxy cinnamic acid -2-fluoro-4-hydroxy- benzonitrile ester and its preparation method
A technology of n-hexyloxyl and liquid crystal compounds, which is applied in the field of replacing cinnamate organic liquid crystal compounds and its preparation, can solve the problems of low viscosity and low working voltage, and achieve high clearing point, wide liquid crystal range and stable chemical properties Effect
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[0015] Implementation 1
[0016] 1) Dissolve 0.01mol p-hydroxycinnamic acid and 0.02mol potassium hydroxide in 40ml of 95% (volume fraction) ethanol, then add 0.03mol of bromo-n-hexane dropwise at a rate of about 1ml / min, reflux for 24h, and then add A 70% (volume fraction) ethanol solution of 0.02mol potassium hydroxide is 14ml, and reflux is continued for 2h. Add 100ml of water, 20ml of concentrated hydrochloric acid, heat for 15min, cool and filter, wash with distilled water, dry, and then recrystallize with 95% (volume fraction) ethanol to obtain p-n-hexoxycinnamic acid, white flake crystals, yield 54 %.
[0017] 2) Add 0.01mol of p-n-hexyloxy cinnamic acid and 20ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve it completely, add 0.01mol of DCC (N,N-diochexylcarbodiimide), wait until turbidity appears After the phenomenon, dissolve 0.01mol 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP [4-(N,N-dimethylamino)pyridine] in 20ml of anhydrous te
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[0018] Implementation 2
[0019] 1) Dissolve 0.02 mol of p-hydroxycinnamic acid and 0.05 mol of potassium hydroxide in 100 ml of 95% (volume fraction) ethanol, then add 0.03 mol of bromo-n-hexane, and reflux for 48 hours. Then add 0.03 mol of potassium hydroxide in 70% (volume fraction) ethanol solution (35 ml), and continue to reflux for 2 hours. 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 p-n-hexoxycinnamic acid, which is white flaky crystals. The yield was 49%.
[0020] 2) Add 0.015mol of p-n-hexyloxy cinnamic acid and 50ml of anhydrous tetrahydrofuran in a three-necked flask, stir to dissolve it completely, add 0.01mol of DCC (N,N-dicyclohexylcarbodiimide), wait until turbidity appears After the phenomenon, 0.015mol of 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP [4-(N,N-dimethylamino)pyridine] were completely di
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