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Preparation process of 3,5-heptadione

A preparation process and heptanedione technology are applied in the field of preparation technology of beta-diketone compounds, and can solve the problems of difficulty in recycling tetrahydrofuran, adverse environmental impact, and high cost, and achieve the solution of difficulty in recycling, lowering production costs, and reducing consumption. Effect

Inactive Publication Date: 2017-06-09
QINGDAO SENMEIKE CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the presence of a large amount of sodium hydride, in actual production, there is a danger because a large amount of sodium hydride is unreacted. In addition, since tetrahydrofuran that is easily soluble in water is used as a solvent, the recovery and utilization of tetrahydrofuran used as a solvent exists. with great difficulty
In addition, a large amount of waste water with high content of organic matter has adverse effects on the environment, and the cost of producing 3,5-heptanedione is also high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Suspend 60g NaH (50%) in 200mL of anhydrous benzene, heat, stir and reflux for 30 minutes, cool down to 60°C, add 2mL of ethanol dropwise, and slowly drop the mixture of 2.5mol ethyl propionate and 1.0mol butanone into the reaction flask In the middle, after adding, react for 2 hours. Then cool down to room temperature, add 200mL of water dropwise under the protection of N2, adjust the pH value to 7.0 with dilute hydrochloric acid, let the reaction solution stand for stratification, separate the organic layer, add 50mL of acetic acid to treat the organic layer, reclaim the solvent, and distill off 3 , 5-heptanedione crude product, 3,5-heptanedione crude product is dissolved in 200ml ethanol, adds the cupric chloride solution 355g of 55g cupric chloride in 300g water to form chelate with 3,5-heptanedione compound, filtered to obtain the copper salt chelate of sky blue 3,5-heptanedione. This chelate compound is dissolved with 1000mL of 20% dilute sulfuric acid, extracted...

Embodiment 2

[0022] Suspend 60g of NaH (50%) in 200mL of toluene, heat, stir and reflux for 30 minutes, cool down to 60°C, add 2mL of methanol dropwise, slowly add the mixture of 2.5mol ethyl propionate and 1.0mol butanone into the reaction flask, After adding, react for 2 hours. Cool down to room temperature, add 200mL of water dropwise under the protection of N2, adjust the pH value to 7.0 with dilute hydrochloric acid, let the reaction solution stand for stratification, separate the organic layer, add 50mL of acetic acid to treat the organic layer, recover the solvent, and evaporate 3 under reduced pressure. The crude product of 5-heptanedione, the crude product of 3,5-heptanedione was dissolved in 200ml ethanol, and 355g of copper chloride solution of 55g copper chloride in 300g water was added to form a chelate with 3,5-heptanedione After filtering, the copper salt chelate of 3,5-heptanedione was obtained. This chelate compound is dissolved with 1000mL of 20% dilute sulfuric acid, ex...

Embodiment 3

[0024] Suspend 60g of NaH (50%) in 200mL of n-hexane, heat, stir and reflux for 30 minutes, cool down to 60°C, add 2mL of methanol dropwise, and slowly drop the mixture of 2.5mol ethyl propionate and 1.0mol butanone into the reaction flask After the reaction was completed for 2 hours, the temperature was lowered to room temperature, and 200 mL of water was added dropwise under the protection of N2, and the pH value was adjusted to 7.0 with dilute hydrochloric acid. Recover the solvent, steam the crude product of 35-heptanedione under reduced pressure, dissolve the crude product of 3,5-heptanedione in 200ml ethanol, add 355g of copper chloride solution of 55g cupric chloride in 300g water to mix with 3,5 -Heptanedione forms a chelate, and is filtered to obtain the copper salt chelate of sky blue 3,5-heptanedione. This chelate compound is dissolved with 1000mL of 20% dilute sulfuric acid, extracted three times with 500ml dichloromethane, the organic layer is dried with anhydrous...

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PUM

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Abstract

The invention discloses a preparation process of 3,5-heptanedione. The process comprises: reacting ethyl propionate with methyl ethyl ketone in the presence of a water-insoluble aprotic solvent to obtain 3,5-heptanedione. The preparation process of 3,5-heptanedione proposed by the present invention uses a water-insoluble aprotic solvent as a reaction solvent, which is easy to recycle and saves production costs.

Description

technical field [0001] The invention relates to a preparation process of a diketone compound, more particularly to a preparation process of a high-purity β-diketone compound. Background technique [0002] In recent years, when ethers and esters of glycols are used as electron donors of olefin polymerization catalysts, catalysts with excellent comprehensive performance can be obtained. When used in propylene polymerization, satisfactory polymerization yield and high stereospecificity can be obtained. At the same time, its 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] 3,5-heptanedione is a key intermediate in the synthesis of 3,5-heptanediol. A method for preparing 3,5-heptanedione has been reported in the literature, but the yield of this method is low and the produ...

Claims

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Application Information

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IPC IPC(8): C07C45/72C07C45/85C07C49/12
CPCC07C45/72C07C45/85
Inventor 李春梅
Owner QINGDAO SENMEIKE CHEM TECH CO LTD
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