Method for synthesizing diaryl acetylene monomer liquid crystal
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A diaryl acetylene and monomer technology, which is applied in the catalytic field of liquid crystal synthesis of diaryl acetylene monomers, can solve the problems of difficult recycling of precious metal catalysts, complicated product purification process, and difficult purification of monomer liquid crystals, etc., and achieves The effect of increasing economic and social benefits, improving synthesis technology, and good catalytic activity
Inactive Publication Date: 2009-09-30
SHIJIAZHUANG CHENGZHI YONGHUA DISPLAY MATERIALS CO LTD
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This traditional homogeneous catalytic reaction system has the following significant disadvantages: since the palladium homogeneous catalyst containing phosphine ligands is mainly used in the current production process, it is difficult to recycle the precious metal catalyst with the product separation in actual production, which not only increases It increases the production cost, causes a lot of waste, and pollutes the environment; in this type of reaction process, different impurity by-products are often produced, and the product purification process is complicated, which brings difficulties to the purification of monomer liquid crystals
There is no report using Pd/C as catalyst in the synthesis of diaryleacetylene monomer liquid crystal
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Embodiment 1
[0055] Embodiment 1——The reaction of propyl cyclohexyl iodobenzene in the mixed solvent of DMF and water
[0056] Add 8.2g (0.025mol) of 4-(4-propylcyclohexyl) iodobenzene, 3.85g (0.0275mol) of 4-methoxyphenylacetylene, 0.05g (0.0003 equivalents) of 5% Pd / C in a 100mL three-necked flask ), CuI 0.1g (0.02 equivalent), PPh 3 0.04g (0.006 equivalent), Et 3 N 8g (3.0 equivalent), DMF 50mL, water 20mL, nitrogen replacement, under the protection of nitrogen, stirred and heated to reflux for 3h, the reaction was completed. Then take a sample for chromatographic analysis, the separation yield: 85%, and the chromatographic purity is 99.6%.
Embodiment 2
[0057] Embodiment 2——The reaction of propyl cyclohexyl iodobenzene in the mixed solvent of acetone and water
[0058] The difference between this example and Example 1 is that the solvent used is a mixed solvent of acetone and water, wherein 50 mL of acetone and 20 mL of water, and other reaction conditions are the same as in Example 1. During the reaction process of this example, a white solid was continuously precipitated. After the reaction was completed, chromatographic analysis was carried out, the separation yield: 90%, and the chromatographic purity: 99.8%.
Embodiment 3
[0059] Embodiment 3 - the reaction of pentyl cyclohexyl iodobenzene in the mixed solvent of acetone and water
[0060] Add 8.9g (0.025mol) of 4-(4-pentylcyclohexyl) iodobenzene, 3.85g (0.0275mol) of 4-methoxyphenylacetylene, 0.05g (0.0003 equivalents) of 5% Pd / C into a 100mL three-necked flask ), CuI 0.1g (0.02 equivalent), PPh 3 0.04g (0.006 equivalent), Et 3 N 8g (3.0 equivalent), acetone 50mL, water 20mL, nitrogen replacement, protection, stirring and heating to reflux for 3h. During the reaction process, a white solid was continuously precipitated, and it was dissolved and sampled for chromatographic analysis. The separation yield was 88%, and the chromatographic purity was 99.6%.
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Abstract
The invention discloses a method for synthesizing a diaryl acetylene monomer liquid crystal, which comprises a method for performing coupling reaction between halogenated aryl hydrocarbon and aryl alkyne, wherein the reaction conditions comprise that the halogenated aryl hydrocarbon and the aryl alkyne perform the coupling reaction in an acetone/water (5:2) solvent at a temperature of between 50 and 110 DEG C, under the normal pressure and under the protection of inert gas, and a catalyst used in the reaction is Pd/C-CuI-PPh3. The halogenated aryl hydrocarbon and the aryl alkyne are added according to an equivalent weight of 1/1.1, three substances in the catalyst Pd/C-CuI-PPh3 are added according to the equivalent weight of (0.0003-0.007)/(0.006-0.05)/(0.005-0.007), and preferentially, the molar percentage of the three substances relative to the halogenated aryl hydrocarbon or the aryl alkyne is 0.03/0.6/0.6. The method can also perform catalytic reaction by using a mother liquor of the filtered product and other solid matters of the coupling reaction to prepare the diaryl acetylene monomer liquid crystal continuously. The method provides a novel catalytic reaction system for synthesizing a diaryl phenylacetylene monomer liquid crystal, the catalyst is cheap and easy to obtain and can be used repeatedly, the separation and purification processes of the liquid crystal product are simple, the products after the reaction are directly filtered out, and the obtained monomer liquid crystal has stable quality and high yield and can greatly reduce the production cost and reduce the waste emission.
Description
technical field [0001] The invention relates to a production method of liquid crystal materials, in particular to a catalytic method for synthesizing liquid crystals of diaryl acetylene monomers. The invention belongs to the technical field of catalytic synthesis chemical industry. Background technique [0002] In order to meet the corresponding characteristics required by various liquid crystal display devices, it is usually necessary to mix and use about 20 kinds of liquid crystal compounds with different properties. According to the use requirements of the display device, the liquid crystal composition should have a suitable optical anisotropy (Δn). In order to shorten the response time of the liquid crystal composition and reduce energy consumption, it is necessary to reduce the driving voltage of the liquid crystal display. In order to achieve a lower driving voltage, the need to increase the dielectric anisotropy Δε. At the same time, in order to meet the fast photoe...
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