Compound, liquid crystal composition and application thereof
A technology of liquid crystal composition and compound, applied in the direction of liquid crystal materials, organic chemistry, chemical instruments and methods, etc., can solve problems such as poor display, achieve moderate optical anisotropy, stable pre-tilt angle, and fast response speed
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Embodiment 1
[0158]
[0159] step 1
[0160]
[0161] Put (0.1mol) 2-bromo-5-chlorophenol and (0.1mol) compound 1 into a 500ml three-necked flask, add 0.15mol anhydrous potassium carbonate, DMF500ml, heat and stir to 90-120°C for 4 hours.
[0162] Add 1000ml of water, separate, wash the organic phase with water, remove the solvent under reduced pressure, dissolve petroleum ether + toluene through a silica gel column, and recrystallize to obtain 35g of white oil (1-a), GC: 99.2%, yield 83%.
[0163] step 2
[0164]
[0165] Dissolve 0.1 mol of compound 2 and 0.1 mol of compound 3 in 500 ml of tetrahydrofuran, then add 0.15 mol of triphenylphosphine, under nitrogen protection, add 0.15 mol of DIAD dropwise, stir at room temperature for 2 hours, add the system to water, wash the organic phase with water, and depressurize The solvent was aliquoted under the following conditions, and toluene+ethanol was recrystallized to obtain 45.1 g of white crystal (1-b), HPLC: 98.7%, yield 74.9%. ...
Embodiment 2
[0186]
[0187] step 1
[0188]
[0189] Add 50g of compound 5 into tetrahydrofuran, under nitrogen protection, cool down to 0°C, add 16g of potassium tert-butoxide in batches, and stir for 30 minutes, dissolve 25g of 2-benzyloxy 5-bromobenzaldehyde in tetrahydrofuran, and add dropwise to in the above system. After the reaction was completed, it was poured into 300 ℃ of water, extracted with ethyl acetate, spin-dried, and separated by column to obtain 35g of white solid 2-a, GC: 98.5%, yield: 90.9%
[0190] step 2
[0191]
[0192] Add 35g of white solid 2-a, 9.6g of potassium acetate, 29.8g of pinacol diborate and 0.5g of tetrakistriphenylphosphopalladium into DMF under nitrogen protection, raise the temperature to 120°C, and keep stirring for 2 hours. The system was poured into water and stirred, extracted with ethyl acetate, the organic phase was washed twice with saturated brine, dried and spin-dried, and 30 g of white solid 2-b was obtained by column separation...
Embodiment 3
[0212]
[0213] step 1
[0214]
[0215] According to the method in step 2 of Example 1, a colorless oil 3-a was obtained, 35 g, GC: 99.1%, yield: 88.1%.
[0216] step 2
[0217]
[0218] According to the method in Step 2 of Example 2, a colorless oily substance 3-b was obtained, 31 g, GC: 98.2%, yield: 82.2%.
[0219] step 3
[0220]
[0221] According to the method in Step 1 of Example 1, a colorless oil 3-c was obtained, 50 g, GC: 97.8%, yield: 85.5%.
[0222] step 4
[0223]
[0224] According to the synthesis method of step 3 of Example 1, 30 g of colorless oil (3-d) was obtained, HPLC: 99.1%, yield 65.5%.
[0225] step 5
[0226]
[0227] According to the synthesis method of step 4 of Example 1, 33 g of compound (3-e) was obtained, HPLC: 99.4%, and the yield was 88.7%.
[0228] step 6
[0229]
[0230] The compound (3-f) 25 g was obtained according to the synthesis method in Step 5 of Example 1, HPLC: 99.1%, and the yield was 89.2%.
[0231] ...
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