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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Embodiment 1
[0016] 1) Dissolve 0.01mol of p-hydroxycinnamic acid and 0.02mol of potassium hydroxide in 40ml of 95% (volume fraction) ethanol, then add 0.03mol of n-bromohexane dropwise at a rate of about 1ml / min, reflux for 24 hours, and then add 0.02mol potassium hydroxide in 70% (volume fraction) ethanol solution is 14ml, 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 p-hexyloxycinnamic acid as white flaky crystals with a yield of 54 %.
[0017] 2) Add 0.01mol of p-hexyloxycinnamic acid and 20ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve it completely, then add 0.01mol of DCC (N,N-Dicordecylcarbodiimide) until turbidity appears After the phenomenon, 0.01mol2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] were dissolved in 20ml of anhydrous tetrahydrofu...
Embodiment 2
[0019] 1) Dissolve 0.02mol of p-hydroxycinnamic acid and 0.05mol of potassium hydroxide in 100ml of 95% (volume fraction) ethanol, then add 0.03mol of n-bromohexane, and reflux for 48h. Then add 35ml of 70% (volume fraction) ethanol solution of 0.03mol potassium hydroxide, and continue to reflux for 2h. Add 100ml of water and 40ml of concentrated hydrochloric acid, mix well, heat for 20min, cool and filter, wash with distilled water, dry, and then recrystallize with 95% (volume fraction) ethanol to obtain p-hexyloxycinnamic acid as white flaky crystals, Yield 49%.
[0020] 2) Add 0.015mol of p-hexyloxycinnamic acid and 50ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.01mol of DCC (N,N-dicyclohexylcarbodiimide) until turbidity appears After the phenomenon, 0.015mol2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] were completely dissolved in 35ml of anhydrous tetrahydrofuran to form a so...
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