Preparation method for ethyl 4-dimethylaminobenzoate

A technology of ethyl dimethylaminobenzoate and dimethylaminobenzoic acid, which is applied in the field of preparation of ethyl p-dimethylaminobenzoate, can solve the problem of high production cost, achieve environmental protection, ensure safety, and be easy to handle. Effect

Inactive Publication Date: 2017-12-05
天津汇仁恒通科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of preparation method of p-dimethylaminobenzoic acid ethyl ester, aim to solve the method production cost that p-dimethylaminobenzoic acid directly carries out esterification preparation p-dimethylaminobenzoic acid ethyl ester in the prior art high problem

Method used

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preparation example Construction

[0027] A preparation method of ethyl p-dimethylaminobenzoate, comprising the following steps,

[0028] (1) Synthesis of p-dimethylbenzoic acid

[0029] The p-dimethylaminobenzaldehyde is fully mixed with the catalyst potassium permanganate under the condition of alkali solution. The addition ratio of p-dimethylaminobenzaldehyde and catalyst potassium permanganate is no more than 2:1, and the catalyst can also be replaced by potassium dichromate. Potassium permanganate and potassium dichromate are used as catalysts compared with silver oxide. The price is low, which greatly reduces the production cost. On the other hand, the oxidizing properties of potassium permanganate and potassium dichromate are stronger than that of silver oxide, and it is easier to oxidize the functional group of the product to carboxylic acid in one step.

[0030] Ensure that the alkali solution is added in a sufficient amount. The alkali solution can be potassium hydroxide or sodium hydroxide or ammoni...

specific Embodiment 1

[0040] A preparation method of ethyl p-dimethylaminobenzoate, comprising the following steps,

[0041] (1) Synthesis of p-dimethylbenzoic acid

[0042] P-dimethylaminobenzaldehyde is fully mixed with the catalyst potassium permanganate in the ratio of 2:1 under the condition of potassium hydroxide solution, wherein the concentration of potassium hydroxide is 7%, so as to ensure that the alkali solution is added in sufficient amount and heated simultaneously , the reaction temperature is controlled at 60°C, and 30 minutes before the reaction is accompanied by stirring. During the stirring process, aluminum oxide powder equivalent to potassium permanganate is slowly added. The total reaction time is controlled at 24 hours. After the reaction is completed, cool the reaction solution to room temperature. ;

[0043] The cooled solution was filtered, and the filtrate was adjusted to neutral or weakly acidic with hydrochloric acid or sulfuric acid, and after a large amount of light ...

specific Embodiment 2

[0051] A preparation method of ethyl p-dimethylaminobenzoate, comprising the following steps,

[0052] (1) Synthesis of p-dimethylbenzoic acid

[0053] P-dimethylaminobenzaldehyde is fully mixed with the catalyst potassium permanganate according to the ratio of 1:1 under the condition of sodium hydroxide, wherein the concentration of sodium hydroxide is 10%, to ensure that the alkali solution is added in sufficient amount, while heating, The reaction temperature is controlled at 65°C, with stirring for 30 minutes before the reaction. During the stirring process, aluminum oxide powder equivalent to potassium permanganate is slowly added. The total reaction time is controlled at 25 hours. After the reaction is completed, cool the reaction solution to room temperature;

[0054] The cooled solution was filtered, and the filtrate was adjusted to neutral or weakly acidic with hydrochloric acid or sulfuric acid, and after a large amount of light yellow precipitates were precipitated,...

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Abstract

The invention provides a preparation method for ethyl 4-dimethylaminobenzoate. The method includes the steps of synthesis of 4-dimethylamino-benzoic acid, synthesis of ethyl 4-dimethylaminobenzoate and the subsequent treatment of the ethyl 4-dimethylaminobenzoate. In the preparation method provided by the invention, a catalyst for converting 4-dimethylaminobenzaldehyde into 4-dimethylamino-benzoic acid is changed into potassium permanganate or potassium dichromate. The method greatly reduces the production cost while guaranteeing the basic yield of the product. In the preparation process, the method avoids using reagents with higher toxicity, especially organic solution, to ensure the safety of the product and provide a guarantee for environmental protection. In addition, the entire production process produces neither overly acid or basic waste water and eases the late treatment of waste water, as well as provides a guarantee for environmental protection.

Description

technical field [0001] The invention belongs to the technical field of producing ethyl p-dimethylaminobenzoate in the chemical industry, in particular to a preparation method of ethyl p-dimethylaminobenzoate. Background technique [0002] Ethyl p-dimethylaminobenzoate is also known as p-N,N-ethyl dimethylaminobenzoate, ethyl 4-dimethylaminobenzoate, photoinitiator EDB, EDB. It is a high-efficiency amine accelerator, often used together with free radical (II) type photoinitiators, mainly used for UV curing of varnish coatings, inks, adhesives, etc. on paper, wood, metal and plastic surfaces. It can also be used for the ultraviolet radiation polymerization of single or multiple monomers, and is a good sensitizer. It is often used in combination with other photoinitiators, which can not only promote photoinitiation, but also eliminate oxygen on the photoinitiator. interference effect. Today, such products have already begun mass production and are put into use in large quanti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/60C07C227/02C07C227/16
CPCC07C227/02C07C227/16C07C229/60
Inventor 穆香田王敬绪
Owner 天津汇仁恒通科技有限公司
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