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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

Inactive Publication Date: 2017-08-01
王志训
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The amination reduction process involved in this synthesis route often requires the use of a large amount of iron powder. In the existing process, such metals are often discarded directly after the reduction is completed, resulting in a large amount of metal pollution and environmental problems.
[0006] In addition, in this synthetic route, the selective acylation process involved often requires precise operation, and a little carelessness will lead to the problem of reduced yield, resulting in an increase in the cost of industrial production

Method used

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Embodiment 1

[0061] The synthetic route involved in this embodiment is as follows:

[0062]

Embodiment 1

[0063] Embodiment one 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 in the pressure reactor -C catalyst 12g (or 15g, 20g, 45g, etc.), after nitrogen protection, replace hydrogen with nitrogen, and react at a temperature of 50°C with a hydrogen pressure of 0.02MPa (0.1MPa, 0.5MPa, 2MPa) for 5 hours ( 1-10 hours); filter to remove insoluble matter, distill methanol and place it for later use. (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 reaction for 2 hours (ranging from 1-8 hours), heat filtration to remove solid residue, distill When there is no distillate, keep it for use.

[0066] (3) Add the above product and 3% Pt-C catalyst (or 15g, 20g, 45g) in the pressure reactor, after ...

Embodiment 1

[0071] Embodiment one B, synthetic route B

[0072] On the basis of the above-mentioned reaction process, in step (1), add 1700g m-dinitrobenzene, zinc powder 250g (or be 300g, 500g, 1000g not etc., or replace iron and aluminium) as in the pressure reactor, Hydroxylamine is obtained under the action of 1200g98% sulfuric acid (or 2300g, 3500g, 4000g), 1000g water (or 5000g, 10000g, 20000g) and carbon dioxide pressure of 0.02MPa (0.1MPa, 0.5MPa, 2MPa). After the product, the insoluble matter was removed by filtration;

[0073] Add 1200g of 98% acetic acid (or 2300g, 3500g, 4000g), 2000g methanol (the amount of the solvent can also be 3200g, 4000g, 5000g, 8000g) to react to obtain amine in the reactor of the above reaction 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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Abstract

The invention provides a disperse dye intermediate preparation method, which is characterized by utilizing m-dinitrobenzene as a raw material and obtaining a target product through amination, amidation and reduction reaction. In addition, the disperse dye intermediate preparation method disclosed by the invention enables waste residues generated in a reaction process to be recycled through a circular metal reduction method. Furthermore, the disperse dye intermediate preparation method disclosed by the invention has environmental friendliness and no pollution.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of a disperse dye intermediate (N-(3-amino-4-methoxyphenyl)acetamide). Background technique [0002] N-(3-amino-4-methoxyphenyl)acetamide is an important intermediate compound for the synthesis of azo dyes and drugs, and is used to synthesize 4-acetamido-2-(N,N-diethanolamino)benzidine Ether, to prepare disperse blue series disperse pigments and disperse dark blue series coupling components, the production and sales volume is very large. [0003] And at present, the synthetic method of N-(3-amino-4-methoxyphenyl) acetamide is varied, mainly uses 2,4-dinitrochlorobenzene as basic raw material to synthesize N-(3-amino-4 -Methoxyphenyl) acetamide, this type of method obtains the target product through methanol etherification, reduction and selective acylation of 2,4-dinitrochlorobenzene. [0004] [0005] The amination reduction process involved in this syn...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C233/43
CPCC07C213/00C07C231/02C07C231/12
Inventor 王志训
Owner 王志训
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