Thiophene derivatives, and lc media containing the same
A technology of liquid crystal media and meaning, applied in the field of thiophene derivatives, can solve problems such as long response time
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Embodiment 1
[0341] Example 1: 2-(4'-ethyl-3-fluorobiphenyl-4-yl)-5-methylthiophene ("PGT-2-1")
[0342] The compound 2-(4'-ethyl-3-fluorobiphenyl-4-yl)-5-methylthiophene ("PGT-2-1") according to the invention was prepared as follows:
[0343]
[0344] 5.0g (28.2mmol) of 2-bromo-5-methylthiophene, 7.70g (28.3mmol) of 4'-ethyl-3-fluoro-4-biphenylboronic acid, 1.70g (1.47mmol) of A mixture of (triphenylphosphine)palladium(0) and 30ml of 2N sodium carbonate solution was heated to reflux for 3h in 90ml of toluene / ethanol (1:2). After cooling, the organic phase was separated and the aqueous phase was extracted several times with toluene. The combined organic phases were washed with water and saturated sodium chloride solution. The solution was dried over sodium sulfate and concentrated completely. The residue was subjected to column chromatography (SiO 2 , n-heptane:toluene=97:3) and purified. Further purification was performed by recrystallization from ethanol and n-heptane; 2-(4'-...
Embodiment 2
[0351] Example 2: 2-(4'-Propyl-3-fluorobiphenyl-4-yl)thiophene ("PGT-3-H")
[0352] The compound 2-(4'-propyl-3-fluorobiphenyl-4-yl)thiophene ("PGT-3-H") according to the invention was prepared as follows:
[0353]
[0354] 25.3g (0.16mol) of 2-bromothiophene, 40.0g (0.16mol) of 4'-propyl-3-fluoro-4-biphenylboronic acid, 8.5g (7.4mmol) of four (triphenylphosphine) ) Palladium (0) mixture and 170ml of 2N sodium carbonate solution in 420ml of toluene / ethanol (1:2) were heated to reflux for 18h. After cooling, the organic phase was separated and the aqueous phase was extracted several times with toluene. The combined organic phases were washed with water and saturated sodium chloride solution. The solution was dried over sodium sulfate and concentrated completely. The residue was subjected to column chromatography (SiO 2 , n-heptane:toluene=9:1) and purified. Further purification is carried out by recrystallization from ethanol and n-heptane; 2-(4'-propyl-3-fluorobiphen...
Embodiment 3
[0361] Example 3: 2-(4'-ethyl-3-fluorobiphenyl-4-yl)-5-propylthiophene ("PGT-2-3")
[0362] The compound 2-(4'-ethyl-3-fluorobiphenyl-4-yl)-5-propylthiophene ("PGT-2-3") according to the present invention was prepared as follows:
[0363] Synthesis of 5-(4'-ethyl-3-fluorobiphenyl-4-yl)thiophene-2-carbaldehyde
[0364]
[0365] 58.5g (0.31mol) of 5-bromothiophene-2-carbaldehyde, 75.5g (0.31mol) of 4'-ethyl-3-fluoro-4-biphenylboronic acid, 17.0g (14.7mmol) of tetrakis( A mixture of triphenylphosphine)palladium(0) and 375 ml of 2N sodium carbonate solution was heated in 935 ml of toluene / ethanol (1:1.5) at 80° C. for 1 h. After cooling, the precipitated product was first dissolved by adding THF. The organic phase was separated and the aqueous phase was extracted with MTBE. The combined organic phases were washed with saturated sodium chloride solution, and the solution was dried over sodium sulfate. The residue remaining after removal of the solvent is soaked in tolu...
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