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New process for synthesizing 1-hydroxycyclohexanecarboxylic acid and application

A technology of hydroxycyclohexylcarboxylic acid and hydroxycyclohexyl, which is applied in the field of synthesizing 1-hydroxycyclohexylcarboxylic acid, can solve the problems of increasing the chance of meeting main and by-products, difficult temperature operation, large heat release of the system, etc., so as to reduce the chance of molecular collision , The effect of controlling the reaction temperature and reducing the reaction temperature

Inactive Publication Date: 2018-12-21
兰博尔开封科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The by-product of this reaction is ammonium chloride. Water is added to the reaction, and the reaction temperature is about 70°C. The entire process environment is particularly conducive to the dissolution of ammonium chloride in the cyclohexanoic acid system, resulting in a large heat release and difficulties for employees to operate the temperature. , and increase the progress of the side reaction, which increases the chance of meeting the main by-products to a greater extent and reduces the yield of this step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A new process for synthesizing 1-hydroxycyclohexyl formic acid: put 210kg of cyclohexanone cyanohydrin and 150kg of cyclohexanone into the acidification kettle in turn, start stirring and pass chlorine, heat is released during the chlorine passage, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the chlorine flow, turn on the reflux, and keep warm at 55°C for 3 hours; after the heat preservation is over, open the cooling water valve to cool the material, and when the temperature drops to 30°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride. The filtrate that is thrown out is 1-hydroxycyclohexyl formic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.

[0031] In this example, the yield of 1-hydroxycyclohexylcarboxylic acid was 87.21%, the purity was 97.11%, the purity of ammonium chloride was 99.21%, and the total yield of spirodic...

Embodiment 2

[0033] A new process for synthesizing 1-hydroxycyclohexyl formic acid: put 240kg of cyclohexanone cyanohydrin and 170kg of cyclohexanone into the acidification kettle sequentially, start stirring and pass chlorine, heat is released during the chlorine passage, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the chlorine flow, turn on the reflux, and keep warm at 50°C for 3.5h; after the heat preservation is over, open the cooling water valve to cool the material, and when the temperature drops to 25°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride , The filtrate thrown out is 1-hydroxycyclohexyl formic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.

[0034] In this example, the yield of 1-hydroxycyclohexylcarboxylic acid was 87.08%, the purity was 97.26%, the purity of ammonium chloride was 99.07%, and the total yield of spirodiclofen...

Embodiment 3

[0036] A new process for synthesizing 1-hydroxycyclohexyl formic acid: put 180kg of cyclohexanone cyanohydrin and 120kg of cyclohexanone into the acidification kettle in turn, start stirring and pass chlorine, heat is released during the chlorine passage, and the temperature in the kettle reaches a maximum of 75 ℃, when the temperature starts to drop, stop the chlorine flow, turn on the reflux, and keep warm at 45°C for 4 hours; after the heat preservation is over, open the cooling water valve to cool the material, and when the temperature drops to 35°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride. The filtrate that is thrown out is 1-hydroxycyclohexyl formic acid, and the centrifuged ammonium chloride is dried and sold as a by-product.

[0037] In this example, the yield of 1-hydroxycyclohexylcarboxylic acid was 87.24%, the purity was 97.46%, the purity of ammonium chloride was 99.42%, and the total yield of spirodic...

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PUM

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Abstract

The invention discloses a new process for synthesizing 1-hydroxycyclohexanecarboxylic acid and an application. During the synthesis of the 1-hydroxycyclohexanecarboxylic acid, an anhydrous system is adopted. According to the process, due to an anhydrous reaction processing technology, a reaction enviroment is improved to the maximum, the progress of a main reaction is improved, adverse factors toreactions caused by a solid-liquid reaction are solved, the reaction yield is increased, and the aftertreatment of salt-bearing compounds becomes more convenient. By using the new process disclosed bythe invention, the yield of the 1-hydroxycyclohexanecarboxylic acid can reach 87% or more, the purity of the 1-hydroxycyclohexanecarboxylic acid can reach 97% or more, the purity of ammonium chloridecan reach 99% or more, and thus, the ammonium chloride can be sold directly as firsts of byproducts; the total yield of spirodiclofen prepared by using the 1-hydroxycyclohexanecarboxylic acid can reach 64% or more. Compared with the traditional processes, the process and the application have the advantages that the whole effect is greatly improved, and the social and economic benefits are huge.

Description

technical field [0001] The invention relates to a new process and application for synthesizing 1-hydroxycyclohexylcarboxylic acid, belonging to the technical field of organic synthesis. Background technique [0002] There are many side reactions in solid-liquid organic synthesis reactions, and the occurrence of side reactions has more or less influence on the main reaction, such as: affecting the progress of the main reaction, affecting the content and yield of the main product, etc. In the process of solid-liquid organic synthesis, salt-containing by-products are the most common. How to solve the problem of salt-containing by-products in the process of solid-liquid organic synthesis has been a research topic for many organic synthesis researchers. [0003] 1-Hydroxycyclohexylcarboxylic acid is a commonly used compound, but during its synthesis, side reactions inevitably occur. The by-product of this reaction is ammonium chloride. Water is added to the reaction, and the rea...

Claims

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Application Information

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IPC IPC(8): C07C51/08C07C62/04C07C51/42C07D307/94
CPCC07C51/08C07C51/42C07D307/94C07C62/04
Inventor 董光霞霍二福常书浩刘沛敬李晓琼乔晓会张玉霞刘宏勋李红金孙宝臣
Owner 兰博尔开封科技有限公司
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