Alkyl dicyclohexyl 2,3-difluorophenylbutenoid liquid crystal compound and application thereof
A liquid crystal compound, difluorophenylbutene technology, applied in liquid crystal materials, organic chemistry, chemical instruments and methods, etc., can solve the problems of low viscosity, low driving voltage, etc., achieve low viscosity, high voltage retention rate, high resistance The effect of rate and dielectric anisotropy
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Embodiment 1
[0040] Embodiment 1. Synthesis of Propylcyclohexylcyclohexenyl 2,3-Difluorobenzene
[0041] Add 94g (0.82mol) 1,2-difluorobenzene, 900ml tetrahydrofuran to a 2L three-necked flask, install a low-temperature thermometer, balloon, dropping funnel, exhaust the air with nitrogen for 5 times, and inject liquid nitrogen outside the bottle to bring the temperature to -60°C , start to drop 0.99mol of butyllithium solution into the bottle, and control the temperature during the dropping process at -60°C to -50°C. 178g, a solution made of propylcyclohexylcyclohexanone and 300ml tetrahydrofuran, the temperature is controlled between -60°C and -50°C during the dropwise addition, and it is kept between -60°C and -50°C for 1 hour after the drop, and then the reaction solution Naturally warm up to room temperature, pour the reaction solution into a hydrolysis bucket containing 1kg ice water and 1L hydrochloric acid under stirring, hydrolyze for 15min, separate the liquids, extract the wate...
Embodiment 2
[0042] Embodiment 2. The synthesis of propyl bicyclohexyl-2,3-difluorobenzene
[0043] Add 256g of propylcyclohexylcyclohexenyl 2,3-difluorobenzene, 500ml of toluene, 200ml of ethanol, 60g of Raney nickel into a 2L bottle, and hydrogenate for 10h under 0.1Mpa atmospheric pressure. The catalyst was filtered off, the solvent was evaporated to dryness, and recrystallized 2-3 times with 1.5 times ethanol to obtain 82 g of the product as white crystals.
Embodiment 3
[0044] Example 3. Synthesis of 4-(propylbicyclohexyl)-2,3-difluorobenzaldehyde
[0045] Add 82g of propylbicyclohexyl 2,3-difluorobenzene and 400ml of tetrahydrofuran to a 1L three-necked flask, blow nitrogen and exhaust the air for 5 times, cool down to -60°C, add 0.27mol of butyllithium solution dropwise, and drop the temperature at -60°C~ Keep at -50°C for 1h, add 25g (0.43mol) dimethylformamide dropwise, exotherm, control the temperature during the dropwise addition at -75°C to -60°C, after dropping, keep at -65°C for 1h, then Naturally raise the temperature to -30°C, pour into a bucket containing 100ml HCl and 100ml water and hydrolyze for 10min, add 1.2L diazomethane and stir, let stand, separate liquids, wash the organic phase with water to be neutral, evaporate the solvent to dryness, and obtain 82g of the product.
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