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Method for preparing m-nitroaniline by m-dinitrobenzene selectivity reduction

A technology for m-dinitrobenzene and nitroaniline, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of pollution selectivity, difficulty in control, etc., and achieves high reduction reaction yield, Low cost and the effect of avoiding pollution problems

Inactive Publication Date: 2008-02-13
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a new method for preparing m-nitroaniline by reducing m-dinitrobenzene with iron powder, aiming at the pollution problem and difficult selectivity control problem in the traditional iron powder-strong acid aqueous reduction system. Traditional strong acid not only has the advantages of iron powder reduction method, but also avoids the pollution of salty wastewater to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 75mL stainless steel autoclave, add 0.42g of m-dinitrobenzene, 0.42g of iron powder, 11.1mL of water, 1.4mL of ethanol, magnets, tighten the autoclave, and use CO 2 Replace the air 5 times, fill it with 2.8MPa carbon dioxide, put it into an 80°C oil bath, start stirring, react for 6 hours to stop the reaction, cool down, release carbon dioxide, extract the product in the kettle with ethyl acetate, analyze the product components by TLC, and use gas phase The content of each component is analyzed by chromatography, and the results show that the conversion rate of m-dinitrobenzene is more than 99%, and the selectivity of m-nitroaniline is more than 99%.

Embodiment 2-10

[0014] Embodiment 2-10, concrete operating conditions see embodiment 1

[0015] implement

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PUM

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Abstract

The invention relates to a preparation method for the m-nitroaniline by selectively deoxidize the m-dinitrobenzene nitrobenzene; the m-dinitrobenzene is used as the raw material and the iron is used as the reductant; with the carbon dioxide / water - ethanol system, the temperature of 40 to 130 Celsius system, and the pressure of 1.6 to 10.0 MPa, the reaction can be done to make the m-nitroaniline; the conversion rate of the reaction is more than 98 percent; the selectivity of the m-nitroaniline is more than 99 percent. In the method of the invention, the carbon dioxide, water, ethanol and the left iron in the reaction can be reused; the invention avoids the problem of the wastewater discharge. At the same time, the invention has the advantages of the high collection rate of the reaction and the good selectivity of the product.

Description

technical field [0001] The invention relates to a method for preparing m-nitroaniline through the selective reduction of m-dinitrobenzene in the fine chemical industry. Background technique [0002] As a large class of important organic synthesis intermediates and raw materials, nitroarylamines are widely used in medicine, pesticides, dyes and other fields. The preparation of nitroarylamines by partial reduction of dinitroaromatic compounds is of great industrial significance. At present, the selective reduction of aromatic dinitro compounds is an important method for the preparation of nitroarylamines, but there are not many methods. The selective reduction methods of dinitro compounds used in industrialization mainly include: sodium sulfide reduction [Xu Kexun. Handbook of Fine Chemical Raw Materials and Intermediates, Beijing: Chemical Industry Press, 2001, 5-531-532], stannous chloride reduction [Wen-Kang Xing and Yoshiro Ogata et al.Effect of Meta and Para Substituent...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 陶源蒋景阳
Owner DALIAN UNIV OF TECH
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