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Preparation method of ethyl nicotinate

A technology of nicotinic acid ethyl ester and nicotinic acid, which is applied in the field of preparation of nicotinic acid ethyl ester, can solve the problems of large loss of anhydrous ethanol and ethyl acetate, increase the cost of wastewater treatment, and high cost, and achieves the reduction of highly polluted wastewater. The effect of producing, suitable for large-scale industrial production, reducing labor and equipment costs

Inactive Publication Date: 2017-07-18
常州沃腾化工科技有限公司
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

The advantage of this process is that the process is relatively simple and the yield is high. The disadvantage is that the loss of anhydrous ethanol and ethyl acetate is large and the cost is high; at the same time, the process will produce a large amount of high-COD and high-sodium sulfate wastewater, which also greatly improves wastewater treatment. The cost is not conducive to large-scale industrial production. The reaction formula is as follows

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0007] In the following examples, the esterification reaction solid acid catalyst is the HND230 solid catalyst produced by Jiangsu Nanda Catalyst Research Center.

[0008] Example 1, in a 500ml four-necked flask, add 123.1g toluene, 92.1g absolute ethanol (2mol), 2.5g solid acid catalyst for esterification reaction and 246.2g nicotinic acid successively, slowly heat up to 55°C, stir and keep warm for reaction 4 hour, then warming up and refluxing for dehydration, the anhydrous reaction is completed, cooled to room temperature, and the solid acid catalyst for the esterification reaction is recovered by filtration, and the filtrate decompresses and reclaims toluene, and the toluene recovery ends to obtain 293.8g of light yellow transparent liquid finished product ethyl nicotinate (GC: 99.5%; Yield: 97.2%).

[0009] Example 2, in a 500ml four-necked flask, add 123.1g toluene, 92.1g absolute ethanol (2mol), the esterification reaction solid acid catalyst and 246.2g nicotinic acid ...

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PUM

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Abstract

The invention relates to a preparation method of ethyl nicotinate. The preparation method is characterized by comprising the following steps of: adding nicotinic acid, absolute ethyl alcohol and an esterification reaction solid acid catalyst into methylbenzene; stirring the mixture to react for 3-6h at 50-65 DEG C; then raising the temperature to return and divide water; finishing the reaction till no water is divided; reducing the temperature to room temperature; filtering and recovering the esterification reaction solid acid catalyst; recovering methylbenzene at a reduced pressure from the filtrate; recovering the methylbenzene to obtain a light yellow transparent liquid which is the finished product ethyl nicotinate, wherein the molar ratio of nicotinic acid and absolute ethyl alcohol is 1: 1 to 1: 2; the weight ratio of nicotinic acid and methylbenzene is 1:0.3 to 1:8; the adding amount of the esterification reaction solid acid catalyst is 0.01-0.1 time of the weight of the nicotinic acid; the esterification reaction solid acid catalyst is an HND230 solid catalyst. The preparation method provided by the invention has the advantages of reducing generation of highly polluted wastewater, reducing the manual and equipment costs and being relatively suitable for industrial production on a large scale.

Description

technical field [0001] The invention relates to a method for preparing ethyl nicotinate, in particular to a method for preparing ethyl nicotinate through a reaction catalyzed by a solid acid catalyst. Background technique [0002] As an important basic chemical raw material, ethyl nicotinate is widely used in the synthesis of medicine and pesticide. At present, the more economical and mainstream synthesis method is to use concentrated sulfuric acid as a catalyst, and carry out esterification reaction between nicotinic acid and absolute ethanol under reflux. PH, then extracted with ethyl acetate, dried over anhydrous sodium sulfate, and distilled off ethyl acetate under reduced pressure. The residue is a light yellow transparent liquid which is the product. The advantage of this process is that the process is relatively simple and the yield is high. The disadvantage is that the loss of anhydrous ethanol and ethyl acetate is large and the cost is high; at the same time, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/80C07D213/803
CPCC07D213/80C07D213/803Y02P20/584
Inventor 万志兵王志超孙克周陈红元
Owner 常州沃腾化工科技有限公司
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