Novel LCD compound p-isoamoxy cinnamic acid -2-fluoro-4-hydroxy- benzonitrile ester and its preparation method
A technology of isopentoxy carbasin and hydroxybenzonitrile, which is applied in chemical instruments and methods, liquid crystal materials, organic chemistry, etc., and can solve problems such as low viscosity and low working voltage
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Embodiment 1
[0015] 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 isopentyl bromide dropwise at a rate of about 1ml / min, reflux for 24 hours, and 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 then recrystallize with 95% (volume fraction) ethanol to obtain p-amyloxycinnamic acid as white flaky crystals. 54%.
[0016] 2) Add 0.01mol of p-amyloxycinnamic acid and 20ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.01mol of DCC (N,N-dicyclohexylcarbodiimide), and wait until After the turbidity phenomenon, 0.01mol2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] were dissolved in 20ml of anhydrous tetrahydrofuran ...
Embodiment 2
[0018] 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 bromoisopentane, and reflux for 48 hours. 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 recrystallize with 95% (volume fraction) ethanol to obtain p-amyloxycinnamic acid as white flaky crystals , yield 49%.
[0019] 2) Add 0.015mol of p-amyloxycinnamic acid and 50ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve it completely, then add 0.01mol of DCC (N,N-dicyclohexylcarbodiimide), and wait until After the turbidity, 0.015mol 2-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 soluti...
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