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Method for preparing 1,4-cyclohexanedione monoethylene glycol ketal

A technology of cyclohexanedione monoethylene glycol ketal and cyclohexanedione, applied in the field of preparation of 1,4-cyclohexanedione monoethylene glycol ketal, which can solve the problems of difficult separation and low conversion rate , to achieve the effect of simple operation, lower reaction cost and less operation steps

Active Publication Date: 2019-03-22
河北彩客新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problems of low conversion rate and difficult separation in the synthesis of existing 1,4-cyclohexanedione monoethylene glycol ketal, the present invention provides a preparation method of 1,4-cyclohexanedione monoethylene glycol ketal , which has a high reaction conversion and product yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 15.2 g of methyltriethylammonium chloride was taken, added to 40.3 g of ethylene glycol, heated to 60° C. to obtain a colorless transparent liquid. 11.2 g of 1,4-cyclohexanedione was weighed and added to the colorless transparent liquid, and reacted at 60° C. for 1 h. After the reaction, it was lowered to room temperature, 35 g of ether was added for extraction, the lower layer solution was taken out, and the solvent was evaporated to obtain 15.1 g of white solid, wherein the content of 1,4-cyclohexanedione monoethylene glycol ketal was 95.7%, and the yield was 92.5%. .

Embodiment 2

[0019] Take 22.7 g of methyltriethylammonium chloride, add it to 46.5 g of ethylene glycol, and heat to 65° C. to obtain a colorless and transparent liquid. The colorless and transparent liquid was cooled to 40 °C, 11.2 g of 1,4-cyclohexanedione was added, and the reaction was carried out at 40 °C for 1.5 h. After the reaction, it was lowered to room temperature, 50 g of ether was added for extraction, the lower layer solution was taken out, and the solvent was evaporated to obtain 15.5 g of white solid, wherein the content of 1,4-cyclohexanedione monoethylene glycol ketal was 94.9%, and the yield was 94.2%. .

Embodiment 3

[0021] 19.7 g of methyltriethylammonium chloride was taken, added to 62 g of ethylene glycol, heated to 50° C. to obtain a colorless transparent liquid. 11.2 g of 1,4-cyclohexanedione was weighed and added to the colorless and transparent liquid, and reacted at 50° C. for 1 h. After the reaction, it was lowered to room temperature, 56 g of ether was added for extraction, the lower layer solution was taken out, and the solvent was evaporated to obtain 15.6 g of white solid, wherein the content of 1,4-cyclohexanedione monoethylene glycol ketal was 96.1%, and the yield was 96.0%. .

[0022] In order to better illustrate the technical solutions of the present invention, further comparisons are made below with the examples of the present invention through comparative examples.

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PUM

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Abstract

The invention relates to the technical field of chemical synthesis and particularly discloses a method for preparing 1,4-cyclohexanedione monoethylene glycol ketal. The method comprises the steps of producing an eutectic system from ammonium methyltriethylchloride and ethylene glycol, and then, directly adding 1,4-cyclohexanedione for a reaction. According to the method disclosed by the invention,produced monoketal is high in selectivity, the yield can reach 90% or more, and other reaction solvents are not required to be used, so that the production cost is reduced; after the reaction ends up, the product is easy to separate, and the operation is simple.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 1,4-cyclohexanedione monoethylene glycol ketal. Background technique [0002] 1,4-Cyclohexanedione monoethylene glycol ketal is an important intermediate for medicine and liquid crystal materials, which is obtained by the condensation of 1,4-cyclohexanedione and ethylene glycol. Since the two carbonyl positions of 1,4-cyclohexanedione are the same and have high reactivity, the condensation reaction will inevitably produce a large number of diketal by-products in addition to the monoketal product, resulting in the conversion rate of the monoketal reaction. And because the properties of 1,4-cyclohexanedione, monoketal and diketal are similar, it is difficult to separate monoketal from the product, and the product yield is low. SUMMARY OF THE INVENTION [0003] Aiming at the problems of low conversion rate and difficult separation in the existin...

Claims

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Application Information

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IPC IPC(8): C07D317/72
CPCC07D317/72
Inventor 孙玉亮邵玉凤崔北文崔凤桐付鹏刘小平司灵敏王淑梅韩俊燕
Owner 河北彩客新材料科技股份有限公司
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