Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation technique of 3,5-heptanedione

A preparation process, the technology of heptanedione, which is applied in 3 fields to achieve the effects of saving production costs, reducing costs and improving safety

Inactive Publication Date: 2012-02-15
淄博润博化工销售有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, in the prior art, there is no known method in which 3,5-heptanedione can be prepared by simple and safe operation at low cost for industrialization, so further improvement is required

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

[0025] In a 1000ml four-neck flask, add 510g of ethyl propionate and 135g of solid sodium methylate, and heat to 70°C under stirring, then add 72g of methyl ethyl ketone within 5 hours with a dropping funnel, and then continue stirring at 70°C React for 5 hours, then lower to room temperature, add 200 g of water dropwise at room temperature, adjust the pH value to 7.0 with dilute hydrochloric acid, leave the reaction solution to separate layers, separate the organic layer, recover ethyl propionate, evaporate 3 under reduced pressure, Crude 5-heptanedione. Gas chromatography analysis confirmed that the crude product contained 51.6 g of 3,5-heptanedione, and the yield was 40%. The crude product of 3,5-heptanedione was dissolved in 150ml of methanol, and 310g of copper nitrate solution of 60g of copper nitrate in 250g of water was added to form a chelate with 3,5-heptanedione, and this chelate was diluted with 15% Sulfuric acid 8000ml dissolves, extracts three times with 300ml d...

Embodiment 2

[0027] The reaction was carried out in the same manner as in Example 1, except that the solid sodium methoxide was changed to 108 g. 49.3 g of crude 3,5-heptanedione was obtained, 46.9 g of purified 3,5-heptanedione, the content was 98.05% (measured by gas chromatography), and the final yield was 35.9%.

Embodiment 3

[0029] The reaction was carried out in the same manner as in Example 1, but the ethyl propionate was changed to 612g to obtain 54.5g of 3,5-heptanedione crude product, and 51.6g of purified 3,5-heptanedione with a content of 97.89% (measured by gas chromatography), final yield 39.46%.

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 belongs to the field of chemical synthesis, and particularly relates to a preparation technique of 3,5-heptanedione, which is characterized in that methylethylketone and ethyl propionate react in the presence of alkali metal alkoxide catalyst to obtain the 3,5-heptanedione without using any solvent. Since no solvent is used, the invention overcomes the defects of wastewater generation and difficulty in recycling when using a solvent, and saves the production cost. In addition, the alkali metal alkoxide is used as the catalyst instead of expensive potassium tert-butoxide, sodium hydride or the like, thereby further lowering the cost and enhancing the production safety. More importantly, since no high-risk hydride is used, the invention prevents danger caused by use of hydride in actual production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation process of 3,5-heptanedione. Background technique [0002] In recent years, when ethers and esters of glycols are used as electron donors for olefin polymerization catalysts, catalysts with excellent comprehensive performance can be obtained. When used in propylene polymerization, satisfactory polymerization effect and high stereospecificity can be obtained. At the same time, the heat sensitivity to hydrogen adjustment is very good, which is beneficial to the development of different types of polymers, especially when used for ethylene-propylene copolymerization, it produces less gel content and has better copolymerization. [0003] At present, the method for preparing 3,5-heptanedione has been reported in the literature, but the yield of this method is low, and the production operability is not strong. [0004] The method using Claisen condensation i...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/12C07C45/45
Inventor 于兵甄美静吴云霞陈立娇谷城张晖耿加强张明明韩涛冯旭高新陈静
Owner 淄博润博化工销售有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com