Liquid crystal compound and liquid crystal medium containing same
A liquid crystal compound and compound technology, which is applied in the preparation of organic compounds, liquid crystal materials, organic chemistry, etc., can solve the problems of few types of VA monomer liquid crystals and the inability to meet the development needs of mixed liquid crystals.
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[0137] R is for C 1 -C 5 straight chain alkyl, C 1 -C 5 straight-chain alkoxy or C 2 -C 5 straight-chain alkenyl, C 2 -C 5 straight-chain alkenyloxy
[0138] "Conventional work-up" means that, if necessary, water is added, the mixture is extracted with dichloromethane, diethyl ether, methyl tert-butyl ether or toluene, the phases are separated, the organic phase is dried and evaporated, and the product is then distilled under reduced pressure or crystallized and / or Or chromatographic purification.
Embodiment 1
[0140]
[0141] Step 1.1
[0142]
[0143] Add 0.9mol chloromethyl ether triphenylphosphonium salt and 1L tetrahydrofuran to a 2L three-necked flask, stir and cool down to 0°C under nitrogen protection, add 1mol potassium tert-butoxide in batches, control the temperature at 0-10°C, and the reaction solution turns reddish brown. After adding potassium tert-butoxide, stir and react for 2 hours, add dropwise 0.8mol cyclopentanone in 100ml tetrahydrofuran solution, control the temperature below 10°C, stir and react for 3 hours after dropping, hydrolyze, separate liquid, extract the aqueous solution twice with 500ml toluene, and combine , wash with water until neutral. Evaporate the solvent to dryness, and distill at atmospheric pressure to obtain the product 0.67mol, GC: 95% yield 83.8%.
[0144] Step 1.2
[0145]
[0146] Add 0.67mol to 1L three-necked bottle 500mL tetrahydrofuran was cooled to 0°C, 200ml concentrated hydrochloric acid and 100ml aqueous solution we...
Embodiment 2
[0165]
[0166] Step 2.1
[0167]
[0168] Add 0.1mol to 1L three-necked bottle 100mL tetrahydrofuran, stirred under nitrogen protection, cooled to -70°C, added 0.11mol n-butyllithium in batches, controlled temperature -70--80°C, dripped butyllithium, stirred for 2 hours, added dropwise 0.2mol of DMF, Control the temperature below -70°C, stir and react for 3 hours after dripping, hydrolyze, separate liquid, extract the aqueous solution twice with 500ml toluene, combine, wash with water until neutral. Evaporate the solvent to get the product 0.08mol, GC: 98%, yield 80%
[0169] Step 2.2
[0170] Add to 500ml three-neck bottle 0.08mol, 200ml tetrahydrofuran, 50ml water, add potassium borohydride 0.1mo 100ml aqueous solution in batches under stirring, and react at room temperature for 4 hours after adding. Add 300ml of dichloromethane, stir, separate the liquids, wash with 200ml of water, perform column chromatography once, and evaporate the solvent to obtain 0.07...
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