Liquid crystal compound containing tetrahydropyrane difluoro methoxy-linking group and preparation method and application thereof
A compound and liquid crystal technology, applied in chemical instruments and methods, organic chemistry, liquid crystal materials, etc., can solve problems such as the space that restricts the improvement of the response speed of liquid crystal mixtures and the significant reduction of the clearing point of liquid crystals.
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Embodiment 1
[0039] Compound I shown in embodiment 1, formula I (R 1 =C 3 h 7 )
[0040]
[0041] step 1
[0042]
[0043] Add 500g (3.73mol) malic acid (I-0) and 500g concentrated sulfuric acid into a 2L three-necked bottle, stir to dissolve the solid, slowly add 300ml (20%) fuming concentrated sulfuric acid dropwise, and finish adding in one hour. After adding, raise the temperature Stir and react at 100°C for 2 hours, cool to room temperature, pour into 2Kg of crushed ice, stir and filter with suction, and wash with water.
[0044] The obtained solid was recrystallized from methanol to obtain 287 g of brown crystal (I-1), yield: 55%
[0045] step 2
[0046]
[0047] Add 100g of brown crystals (I-1), 200ml of toluene, 100ml of methanol, and 20g of Raney nickel catalyst into a 2L single-necked bottle, shake and hydrogenate at room temperature and pressure for 6 hours, absorb hydrogen to the theoretical amount, carefully filter to remove the catalyst, and depressurize the fil...
Embodiment 2
[0070] Embodiment 2, compound I45 shown in preparation formula I (R 1 =C 3 h 7 )
[0071]
[0072] step 1
[0073]
[0074] Add 286g (1.1mol) 2,3',4',5',6-pentafluoro-[1,1'-biphenyl]-4-phenol and 131.5g (1.3mol) triethylamine into a 5L three-necked flask, Put 1500ml of dichloromethane in a low-temperature tank, cool down to -80°C, add dropwise I-3 and 1000ml of dichloromethane solution prepared in step 3 of Example 1, add it in 3 hours, and after 1 hour, it is still at -80°C Add 515ml of pyridine hydrogen fluoride (70%, 4mol) solution dropwise, and finish adding in half an hour, then add dropwise 640g (4mol) of bromine and 500ml of dichloromethane solution at -80°C, keep stirring and react for 2 hours after adding, remove the low temperature tank , naturally rise to room temperature, add 32% sodium hydroxide aqueous solution (adjust the pH value to 5-8) and 1000g ice, extract the aqueous phase with 200ml dichloromethane after liquid separation, combine the organic ph...
Embodiment 3
[0092] Embodiment 3, compound I29 shown in preparation formula I (R 1 =C 5 h 11 )
[0093]
[0094] step 1
[0095]
[0096] Add 38.7g (0.16mol) 3-fluoro-4'-pentyl-1,1'-biphenyl and 250ml tetrahydrofuran into a 500ml three-necked flask, place it in a low-temperature tank under a nitrogen atmosphere, cool down to -80°C, drop Add 70.5ml (2.5M, 0.176mol) of n-butyllithium hexane solution, and complete the addition in 1 hour. After 1 hour, transfer to a constant pressure dropping funnel;
[0097] Add 39.5g (0.13mol) (I-5) prepared in Step 1 of Example 2 and 200ml tetrahydrofuran solution to a 1L three-necked flask, stir to dissolve and clear, place in a low-temperature tank under a nitrogen atmosphere, cool to -10°C, drop Add the above-prepared 2-fluoro-4-(4'-pentyl-phenyl)phenyllithium tetrahydrofuran solution, and complete the addition in 2 hours. After 1 hour, remove the low-temperature tank, let it rise to room temperature naturally, and add 100ml of saturated ammoni...
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