Liquid crystal compound 4'-n-decyloxy-4-phenylazobenzoic acid-3-fluoro-4-cyanobenzene ester and preparation method thereof
A technology of azobenzene carboxylic acid and liquid crystal compound, applied in the field of organic synthesis, can solve problems such as low working voltage and low viscosity, and achieve the effects of high clearing point, stable chemical properties and wide liquid crystal range
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Embodiment 1
[0015] 1) Dissolve 0.01mol p-hydroxyazobenzenecarboxylic acid and 0.02mol potassium hydroxide in 60ml 95% (volume fraction) ethanol, add 0.03mol brominated decane dropwise at a speed of about 1ml / min, and reflux reaction After 24 hours, add 20 ml of 0.02 mol potassium hydroxide in 70% (volume fraction) ethanol solution, and continue to reflux for 2 hours. 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 4'-n-decyloxy-4-azobenzenecarboxylic acid, It is orange-red flaky crystal, and the yield is 50%.
[0016] 2) Add 0.01mol of 4'-n-decyloxy-4-azobenzenecarboxylic acid and 20ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.01mol of DCC (N,N-dicyclohexyl Carbodiimide), after turbidity appears, dissolve 0.01mol 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)p...
Embodiment 2
[0018] 1) Dissolve 0.02mol of p-hydroxyazobenzenecarboxylic acid and 0.05mol of potassium hydroxide in 50ml of 95% (volume fraction) ethanol, then add 0.06mol of iodo-n-decane, and reflux for 60h. Then add 45 ml of 0.07 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 4'-n-decyloxy-4-azobenzene Carboxylic acid, orange-red flaky crystals, yield 48%.
[0019] 2) Add 0.015mol of 4'-n-decyloxy-4-azobenzenecarboxylic acid and 50ml of anhydrous tetrahydrofuran into a three-necked flask, stir to dissolve completely, then add 0.01mol of DCC (N,N-dicyclohexyl Carbodiimide), after turbidity appeared, 0.015mol 2-fluoro-4-hydroxybenzonitrile and a small amount of DMAP[4-(N,N-dimethylamino)pyridine] were completely dissolved in 35ml anhydrous...
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