Preparation method of C5 side chain substituted fluorine-containing diamine monomer
A fluorine-containing diamine and monomer technology, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc. Difficulties and other problems, to achieve the effect of improving light transmittance, high synthesis yield, and reducing order and symmetry
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[0026] Example 1
[0027] Step 1: Add 1.2L DMAC, 1000g 2,2-bis(3-amino-4-phenol sodium phenol) hexafluoropropane and 732g bromo C5 alkane to a 10L four-necked reaction flask, turn on stirring and heating, and maintain React at 80°C for 2-3h. After the reaction of the raw materials, turn off the heating, pour out the reaction solution, and filter while it is hot. The upper filter cake is the by-product sodium bromide, which is collected and stored. The filtrate is naturally cooled to room temperature, and then added to 2.4 After quenching in L water, there will be a large amount of solids appearing at this time, suction filter, and then wash the filter cake with 3.5L of water, after pumping dry, the filter cake is vacuum dried to obtain 1111g of pure C5-FN.
[0028] Step 2: Add 1111g C5-FN and 550mL NMP into a 10L four-necked reaction flask, turn on the stirring, and then slowly drop a mixture of 812g m-nitrobenzoyl chloride and 550mL NMP into it, and control the reaction liquid dur...
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[0030] Example 2
[0031] The first step: Add 24.3L DMAC, 1000g 2,2-bis(3-amino-4-sodium phenolate) hexafluoropropane and 3658g bromo C5 alkane to a 30L double-layer glass reactor, turn on stirring and heating, Keep at 166℃ for 2-3h. After the reaction of the raw materials, turn off the heating, release the reaction liquid, and filter while it is hot. The upper filter cake is the by-product sodium bromide, which is collected and stored. The filtrate is naturally cooled to room temperature, and then added to 48.6 After quenching in L water, there will be a large amount of solids appearing at this time, suction filter, and then wash the filter cake with 3.5L water, after pumping dry, the filter cake is vacuum dried to obtain 1173g of pure C5-FN.
[0032] Step 2: Add 1173g C5-FN and 11.5L NMP to the 30L double-layer glass reactor, turn on the stirring and jacket to cool down, when the temperature of the reaction liquid drops to 0℃, slowly add 4286g m-nitrobenzene dropwise to it For t...
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