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A kind of preparation method of 4-chloro-2,5-dimethoxyaniline

A technology of dimethoxyaniline and oxygen, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, chemical instruments and methods, etc., can solve problems such as environmental pollution and inconformity with the concept of green development, and achieve the effect of reducing costs

Active Publication Date: 2022-03-18
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above chlorination process such as chlorine chlorination has a certain risk
In addition, the nitrification step produces a large amount of waste water, and the large amount of iron sludge and waste water generated in the reduction step cause a large amount of environmental pollution, which is not in line with the current green, safe and environmentally friendly development concept

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method of 4-chloro-2,5-dimethoxyaniline, comprising the steps of:

[0016] Add 10.17g (80mmol) of 9N hydrochloric acid into a 25ml reaction flask, add 1.53g (10mmol) of 2,5-dimethoxyaniline, add 3.4g (20mmol) of copper chloride, raise the temperature to 95°C, and feed oxygen for 8h . After the reaction was completed, cool to room temperature and filter. After the filter cake was alkalized, 1.81 g of crude product was obtained by filtration. HPLC analysis showed a conversion rate of 100% and a selectivity of 95%. The crude product was rectified under reduced pressure to obtain 4-chloro-2,5-di Methoxyaniline 1.78g (9.5mmol), purity 98.85% (HPLC), yield: 94.93%.

Embodiment 2

[0018] A preparation method of 4-chloro-2,5-dimethoxyaniline, comprising the steps of:

[0019] Add 10.17g (80mmol, containing 3.4g (20mmol) of copper chloride) of concentrated mother liquor 9N hydrochloric acid to a 25ml reaction flask, add 1.53g (10mmol) of 2,5-dimethoxyaniline, raise the temperature to 95°C, and Into oxygen, reaction 8h. After the reaction was completed, cool to room temperature and filter, and then filter the cake after alkalization to obtain 1.8 g of crude product. According to HPLC analysis, the conversion rate was 100%, and the selectivity was 94.76%. The crude product was rectified under reduced pressure to obtain 1.778 g (9.48 mmol) of 4-chloro-2,5-dimethoxyaniline, with a purity of 98.63% (HPLC), and a yield of 94.83%.

[0020] In order to better illustrate the technical solution of the present invention, a further comparison is made below through comparative examples and examples of the present invention.

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PUM

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Abstract

The invention discloses a preparation method of 4-chloro-2,5-dimethoxyaniline, which belongs to the field of chemical synthesis. The method uses 2,5-dimethoxyaniline as a raw material, copper chloride as a reaction system catalyst, and reacts at 95° C. for 8 hours by passing oxygen into a 9N hydrochloric acid solution. After the reaction is completed, cool to normal temperature and filter, and the filter cake is alkalized and filtered to obtain the crude product. The conversion of this reaction was 100% with a selectivity of 95%. After the crude product was purified by vacuum distillation, the product content was 98.85%, and the yield was 94.93%.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of 4-chloro-2,5-dimethoxyaniline. Background technique [0002] 4-Chloro-2,5-dimethoxyaniline is the main raw material for the synthesis of naphthol AS-IRG and naphthol AS-LC. It is an important fine chemical organic pigment intermediate, and the downstream high-end pigment products extended from it Pigment yellow 49, 83, 97, 176, pigment red 146, 184, etc., are mainly used in paint, printing ink, viscose fiber, fabric printing and dyeing (wallpaper, etc.), organic plastic coloring and other fields, and have a wide range of applications in daily production and life. It is an organic chemical raw material whose market demand has increased year by year in recent years. At present, the synthesis of 4-chloro-2,5-dimethoxyaniline is mainly based on hydroquinone as a raw material through alkylation to obtain p-xylylene dimethyl ether, and then nitrate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/08C07C217/84
CPCC07C213/08C07C217/84
Inventor 邱滔陈吉之吕新宇
Owner CHANGZHOU UNIV
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