Preparation method of 4-iodobiphenyl

A technology of iodine biphenyl and biphenyl, which is applied in the field of organic chemical synthesis, can solve the problems of no high-purity 4-iodine biphenyl, difficulty in synthesizing 4-iodine biphenyl, and difficulty in replacing only iodine ions, and reduce energy consumption. , the effect of shortening the reaction time and reducing the production cost

Inactive Publication Date: 2015-06-24
XUCHANG HAOFENG CHEM TECH
3 Cites 1 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Compared with 4,4-diiodobiphenyl, the synthesis of high-purity 4-iodobiphenyl is very difficult
Because the 8-position of biphenyl and the 8-position of 4-iodobiphenyl are almost the same in activity, it is difficult to ensure that the iodide ion only replaces one hydrogen in the reaction, that is, i...
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Abstract

The invention provides a preparation method of 4-iodobiphenyl, belonging to the field of organic chemical synthesis. According to the preparation method, the technical problems that a product of a traditional synthesis method is low in purity, poor in appearance and color and tedious and complex to separate and purify are solved. By virtue of the method for synthesizing high-purity 4-iodobiphenyl by introducing a novel Cu-La silicon dioxide mesoporous composite catalyst into iodination reaction of biphenyl, the technical problems are solved. A new method having the advantages of low cost and pollution and high purity and selectivity is provided for the industrial production of liquid crystal material intermediate 4-iodobiphenyl.

Application Domain

Halogenated hydrocarbon preparation

Technology Topic

4-iodobiphenylChemistry +7

Examples

  • Experimental program(4)

Example Embodiment

[0016] Example 1
[0017] Add 14.52g biphenyl, 11.42g iodine, 272ml acetic acid, 1.22ml concentrated sulfuric acid, 3ml concentrated nitric acid, and 3g Cu-La composite mesoporous SiO in a 500ml reaction flask at room temperature. 2 Slowly raise the temperature to 70°C to start the reaction, control the reaction temperature to 70°C, take a sample of GC and detect that there is no biphenyl in the reaction solution, then continue to stir the reaction for 25 minutes to stop heating; lower the temperature to 40°C, discharge cooling, and centrifuge The crude product is obtained, activated carbon is added to the crude product for decolorization, left to stand, recrystallized with ethyl acetate, filtered and dried to obtain 20.33 g of a pure white product with a purity of 99.5%.

Example Embodiment

[0018] Example 2
[0019] Add 14.52g biphenyl, 9.13g iodine, 230ml acetic acid, 1.22ml concentrated sulfuric acid, 3ml concentrated nitric acid, 3.5g Cu-La composite mesoporous SiO in a 500ml reaction flask at room temperature. 2 Slowly raise the temperature to 75°C to start the reaction. Control the reaction temperature to 75°C. After sampling the GC to detect that there is no biphenyl in the reaction solution, continue to stir the reaction for 20 minutes to stop heating; lower the temperature to 40°C, discharge cooling, and centrifuge The crude product is obtained, activated carbon is added to the crude product for decolorization, left standing, recrystallized with ethyl acetate, filtered and dried to obtain a pure white product 16.25 with a purity of 99.5%.

Example Embodiment

[0020] Example 3
[0021] Add 14.52g biphenyl, 13.70g iodine, 300ml acetic acid, 1.22ml concentrated sulfuric acid, 3ml concentrated nitric acid, and 3.8g Cu-La composite mesoporous SiO in a 500ml reaction flask at room temperature. 2 Slowly raise the temperature to 80°C to start the reaction, control the reaction temperature to 80°C, take a sample of GC and detect that there is no biphenyl in the reaction solution, then continue to stir the reaction for 15 minutes to stop heating; cool to 40°C, discharge cooling, centrifuge and filter The crude product is obtained, activated carbon is added to the crude product for decolorization, left standing, recrystallized with ethyl acetate, filtered and dried to obtain a white pure product 21.32 with a purity of 99.5%.

PUM

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Description & Claims & Application Information

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