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P-aminoanisole electrochemical synthesis method

A technology for p-aminoanisole and a synthesis method, applied in the field of electrochemistry, can solve the problems of harsh reaction conditions, high price, harsh reaction conditions and the like, and achieves the effects of mild reaction conditions, easy reaction and small scale effect.

Inactive Publication Date: 2008-05-28
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The p-nitroanisole reduction method uses sodium sulfide, hydrazine hydrate, etc. as catalysts, and a large amount of lye, sulfur-containing wastewater, etc. are produced, causing serious pollution to the environment; or expensive precious metal catalysts are used, and the reaction conditions are harsh
[0004] The traditional synthesis method of p-aminoanisole either uses expensive noble metal catalysts, or produces a large amount of waste during the reaction process, or requires harsh reaction conditions. Therefore, the traditional production method has no great development prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the second step, take 20ml of methanol and 10ml of 1.5mol / L sulfuric acid solution and mix it into 30ml of methanol-sulfuric acid solution, add 0.3063g of p-nitroanisole, which is 0.00201mol, that is, add 0.067mol per liter of methanol-sulfuric acid solution The p-Nitroanisole, make catholyte, get 20ml methyl alcohol and the sulfuric acid solution of 10ml 1.5mol / L and mix into the methyl alcohol-sulfuric acid solution of 30ml, as anolyte; In the 3rd step, constant voltage is-0.4V, The amount of electricity is 1164c, which is equivalent to 6F per mol of p-nitroanisole; in the fourth step, the yield is 40.7%.

Embodiment 2

[0024] In the second step, take 20ml of methanol and 10ml of 1.5mol / L sulfuric acid solution and mix it into 30ml of methanol-sulfuric acid solution, add 0.3063g of p-nitroanisole, which is 0.00201mol, that is, add 0.067mol per liter of methanol-sulfuric acid solution The p-Nitroanisole, makes catholyte, gets 20ml methyl alcohol and the sulfuric acid solution of 10ml 1.5mol / L and mixes the methyl alcohol-sulfuric acid solution of 30ml, as anolyte; In the 3rd step, constant voltage is-0.5V, The amount of electricity is 1164c, which is equivalent to 6F per mol of p-nitroanisole; in the fourth step, the yield is 13.8%.

Embodiment 3

[0026] In the second step, take 22.5ml of methanol and 7.5ml of 2.0mol / L sulfuric acid solution and mix them into 30ml of methanol-sulfuric acid solution, add 0.3063g of p-nitroanisole, which is 0.00201mol, that is, every liter of methanol-sulfuric acid solution adds The p-Nitroanisole of 0.067mol makes catholyte, gets the methyl alcohol-sulfuric acid solution of 22.5ml methyl alcohol and 7.5ml 2.0mol / L to be mixed into the methanol-sulfuric acid solution of 30ml, as anolyte; In the 3rd step, constant voltage is -0.5V, the electric current is 1164c, which is equivalent to 6F per mol of p-nitroanisole; in the fourth step, the yield is 63.3%.

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Abstract

Provided is an electrochemical synthetic method of aminoanisole, belonging to the technical field of electrochemistry. The method needs to be accomplished in a two-chamber electrolysis bath which is separated by employing a cation-exchange membrane, a copper sheet is taken as a negative electrode, a ruthenium net is taken as a positive electrode, a saturated calomel electrode is taken as a reference electrode, the negative electrode and the reference electrode are installed inside a cathode chamber of the electrolysis bath, and the positive electrode is installed inside an anode chamber of the electrolysis bath. Methanol is taken as solvent, sulphuric acid is taken as supporting electrolyte, paranitroanisole is taken as electrolytic reaction substrate, the solvent and the solution of supporting electrolyte are injected into the cathode chamber and the anode chamber, and the electrolytic reaction substrate is injected into the cathode chamber. The electrolyzation is performed within a condition of normal temperature and pressure and a condition that the negative electrode is added with a certain constant voltage relative to the reference electrode, and the constant voltage is between -0.4 to -0.6 V. After the electrolyzation is finished, the electrolyte is post-processed to obtain the product of paraphenetidine with the production ratio between 24.5-63.3%. The method has the advantages of simple requirement, mild reaction conditions, easy preparation of the electrodes, low price, small pollution in the process of reaction and the like, and is a greening production line.

Description

technical field [0001] The invention relates to an electrochemical synthesis method of p-aminoanisole, which belongs to the technical field of electrochemistry. Background technique [0002] P-aminoanisole, also known as p-methoxyaniline, commonly known as p-anisidine, molecular formula C 7 h 9 NO, white crystal, melting point 57.2°C, boiling point 243°C, relative density 1.071, refractive index 1.5559 (57°C), easily soluble in ethanol, methanol, benzene, ether and chloroform, hardly soluble in water. p-Aminoanisole is mainly used in the dye industry to prepare ice dyes, disperse dyes, vat dyes, cationic dyes, chromophores and naphthols, etc. In the pharmaceutical industry, it is used to produce adipine, primaquine, indomethacin Wait. [0003] The existing methods for producing p-aminoanisole are mainly organic synthesis methods, including 1. Nitrobenzene method, at 75-125°C and 0.6-1.5MPa, using precious metals as catalysts, sulfuric acid, methanol or dimethyl Sulfoxide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/04C25B3/25
Inventor 陆嘉星薛腾柳英姿林美玉张凯杜艳芳
Owner EAST CHINA NORMAL UNIV
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