Disperse dye intermediate preparation method
A technology for disperse dyes and intermediates, applied in the preparation of organic compounds, the preparation of carboxylic acid amides, chemical instruments and methods, etc., can solve the problems of rising industrial production costs, reduced yields, metal pollution, etc. The effect of less impurities and less side reactions
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[0060] Example one
[0061] The synthetic route involved in this example is as follows:
[0062]
Example Embodiment
[0063] Example 1 A, synthetic route A
[0064] (1) Add 1700g m-phenylenedinitro, 2000g methanol (the amount of the solvent can also be 3200g, 4000g, 5000g, 8000g), 600-1200g strong acid ion exchange resin, 3% Pt into the pressure reactor -C catalyst 12g (or 15g, 20g, 45g, etc.), after nitrogen protection, replace the hydrogen with nitrogen, and react for 5 hours at a temperature of 50°C and a hydrogen pressure of 0.02MPa (0.1MPa, 0.5MPa, 2MPa, etc.) ( 1-10 hours); filter to remove insoluble materials, distill methanol and place for later use. (The ion exchange resin removed by filtration can be recycled)
[0065] (2) After cooling, add 1000g of acetic anhydride (the amount of acetic anhydride can also be 2000g, 2500g, 3000g, 4000g), reflux for 2 hours (ranging from 1-8 hours), hot filter to remove solid residue, and distill Set aside until there is no fraction.
[0066] (3) Add the above product, 3% Pt-C catalyst (or 15g, 20g, 45g, etc.) into the pressure reaction vessel. After ni...
Example Embodiment
[0071] Example one B, synthetic route B
[0072] On the basis of the above reaction process, in step (1), for example, add 1700g m-dinitrobenzene and 250g zinc powder (or 300g, 500g, 1000g, or replace with iron and aluminum) into the pressure reactor, Hydroxylamine can be obtained under the action of 1200g 98% sulfuric acid (or 2300g, 3500g, 4000g range), 1000g water (or 5000g, 10000g, 20000g range) and carbon dioxide pressure 0.02MPa (0.1MPa, 0.5MPa, 2MPa range) After the product, filter to remove insoluble materials;
[0073] Add 1200g 98% acetic acid (or 2300g, 3500g, 4000g, etc.), 2000g methanol (the amount of the solvent can also be 3200g, 4000g, 5000g, 8000g) in the above reaction kettle to react to obtain amine Chemical intermediate products.
[0074] It is worth noting that in the above two types of embodiments, when aluminum, zinc or iron is used as the reducing agent, after the reaction, the pH of the reaction solution is adjusted to precipitate metal ions, and after filt...
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