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Method for preparing lignocaine ethyl ester caproic acid by catalyzing cation exchange resin in type of sulfonic acid

A technology of diethylaminoethyl hexanoate and cation exchange, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of high consumption of acyl chloride method, excessive three wastes, etc., and achieve non-corrosiveness , The effect of improving economic benefits and simple operation process

Inactive Publication Date: 2008-06-11
天津市施普乐农药技术发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems existing in the above-mentioned technology, the purpose of this invention is to provide a kind of method that sulfonic acid type cation exchange resin catalyzes and prepares diethylaminoethyl hexanoate, and this method can improve reaction yield, can avoid making impurity again The trouble of too much acid and the high consumption of the acid chloride method, the problem of too many wastes

Method used

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  • Method for preparing lignocaine ethyl ester caproic acid by catalyzing cation exchange resin in type of sulfonic acid
  • Method for preparing lignocaine ethyl ester caproic acid by catalyzing cation exchange resin in type of sulfonic acid
  • Method for preparing lignocaine ethyl ester caproic acid by catalyzing cation exchange resin in type of sulfonic acid

Examples

Experimental program
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Embodiment 1

[0026] The 100ml four-necked bottle is equipped with a stirrer, and a water separator is equipped under the reflux condenser. Put in 23.6g of hexanoic acid, 21.06g of diethylaminoethanol, 30ml of toluene, and 0.4g of domestic brand strong acid-1 resin (hydrogen type, air-dried) about 1.9%, slowly heated to reflux, and kept at reflux for 4 to 10 hours. When the water separator no longer separates water, the reaction is over. Separate resin, remove solvent, rectify, collect 88~90 ℃ / 1mmHg diethylaminoethyl hexanoate product, obtain the diethylaminoethyl hexanoate of 37.5g colorless oily liquid, the chromatographic analysis purity is 96%.

Embodiment 2

[0028] The experimental device and operation were the same as in Example 1, and 0.8 g of hydrogen-form wet resin was used as a catalyst at about 1.9% to obtain 36.7 g of the product diethylaminoethyl hexanoate with a purity of 95%.

Embodiment 3

[0030] The experimental apparatus and operation were the same as in Example 1, and the catalyst was concentrated sulfuric acid to obtain 34.6 g of diethylaminoethyl hexanoate product with a purity of 95%.

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Abstract

This invention provides a method for preparing diethylaminoethyl hexanoate with sulfonic acid-type cation exchanger resin as the catalyst. The method comprises: (1) selecting n-hexanoic acid and diethylaminoethanol as the raw materials at a mol. ratio of (1.1-1.3):1,0; (2) selecting crosslinked polystyrene sulfonic acid-typed cation exchange resin as the catalyst for esterification; (3) adding the raw materials to a reactor, stirring, heating to refluxing, and removing water in the water segregator below the refluxing condenser till no water is formed; (4) separating the resin, removing the solvent, and distilling to obtain the final product. The method has such advantages as high product yield (90-93%), high product purity (95-96%), simple operation, no corrosion, low raw material consumption, and high profit. After application, the crops yield can be increased by 10-50%, and even 50-80% for capsicum, tomato, etc.

Description

technical field [0001] The present invention relates to an agricultural phytohormone synthesized by a chemical method, in particular to a sulfonic acid type cation exchange resin used for various crops such as vegetables, fruits, cotton, and rice, which can promote crop development, disease resistance, and yield increase Catalyzed method for preparing diethylaminoethyl hexanoate. Background technique [0002] According to reports, most of the synthesis methods of diethylaminoethyl hexanoate are direct esterification of hexanoic acid and diethylaminoethanol, using concentrated sulfuric acid as a catalyst. ZL-92112507.0 literature report used titanium dioxide or heteropolyacid as catalyst. Concentrated sulfuric acid is a classic esterification catalyst, and its disadvantage is that the yield is not high, generally 80-85%. The activity of this reaction is reduced due to the salt formation of sulfuric acid and diethylaminoethanol, and the production of heteropolyacid is troubl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C219/06C07C213/06B01J31/10
Inventor 苏荫田胡敏马锦明葛雅琴焦兰瑾
Owner 天津市施普乐农药技术发展有限公司