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
View PDF11 Cites 2 Cited by
  • 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, th

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap