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Synthetic method of 4-R-3,5-heptadione

A synthetic method, the technology of heptanedione, which is applied in the field of chemical synthesis, can solve the problems of high cost, low product yield, and difficult recycling of solvents, etc., and achieve the effects of short reaction cycle, high yield, and easy control of reaction conditions

Inactive Publication Date: 2012-05-02
淄博德丰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the above-mentioned method paths all need complex chemical operations, the solvent is not easy to recycle, and the cost is high, and the yield of the final product is very low. According to relevant literature reports, 4-R-3,5-heptanedione The product yield is about 40%

Method used

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  • Synthetic method of 4-R-3,5-heptadione

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Suspend 85g of sodium ethylate with a mass fraction of 90% in 200ml of benzene in a reaction flask, add 1.2mol of 3,5-heptanedione dropwise into the reaction flask, react for 1 hour and cool to room temperature, add 1.5mol of bromoethane Then, react for 3 hours. After the reaction was completed, the pH value was adjusted to 7.0 with dilute hydrochloric acid, the reaction solution was allowed to stand and separated, and the organic layer was separated. The organic layer was dried with anhydrous sodium sulfate, and the solvent was recovered to finally obtain 0.66 mol of the product 4-ethyl-3,5-heptanedione with a yield of 55%.

Embodiment 2

[0018] Suspend 85g of sodium ethoxide with a mass fraction of 90% in 200ml of toluene in a reaction flask, add 1.2mol of 3,5-heptanedione dropwise into the reaction flask, react for 1 hour and cool to room temperature, add 1.5mol of bromoethane Then, react for 3 hours. After the reaction was completed, the pH value was adjusted to 7.0 with dilute hydrochloric acid, the reaction solution was allowed to stand and separated, and the organic layer was separated. The organic layer was dried with anhydrous sodium sulfate, and the solvent was recovered to finally obtain 0.624 mol of the product 4-ethyl-3,5-heptanedione with a yield of 52%.

Embodiment 3

[0020] Suspend 85g of sodium ethoxide with a mass fraction of 90% in 200ml of xylene in a reaction flask, add 1.2mol of 3,5-heptanedione dropwise into the reaction flask, react for 1 hour and cool to room temperature, add 1.5mol of ethyl bromide After alkane, react for 3 hours. After the reaction was completed, the pH value was adjusted to 7.0 with dilute hydrochloric acid, the reaction solution was allowed to stand and separated, and the organic layer was separated. The organic layer was dried with anhydrous sodium sulfate, and the solvent was recovered to finally obtain 0.636 mol of the product 4-ethyl-3,5-heptanedione with a yield of 53%.

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a synthetic method of 4-R-3,5-heptadione. The method is characterized in that: 3,5-heptadione undergoes a reaction with halogenated hydrocarbon in the presence of an aprotic solvent to obtain 4-R-3,5-heptadione. The method has the advantages that: the aprotic solvent is taken as a reaction solvent, so that recovery is easy, the cost is saved greatly, the synthetic method is easy, convenient and practical, and the yield of the obtained 4-R-3,5-heptadione is high.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of 4-R-3,5-heptanedione. Background technique [0002] Ethers and esters of diols, as catalysts for olefin polymerization, have excellent catalytic effects, especially when used for propylene polymerization, with high polymerization yields. [0003] For, 4-R-3,5-heptanedione is a key intermediate for the synthesis of 4-R-3,5-heptanediol. [0004] It is known that the hydrogen on the active methylene in the β-diketone compound is easily captured by the base to become a monovalent carbanion, and the carbanion undergoes a substitution reaction with the haloalkane, and the final result is that the hydrogen on the active methylene is replaced by the alkane Substituting the base produces an alkylated product. As shown in the following formula: [0005] [0006] However, the above-mentioned method paths all need complex chemical operations, the solv...

Claims

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Application Information

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IPC IPC(8): C07C45/68C07C49/12C07C49/213
Inventor 陈立娇甄美静张晖耿加强于兵谷城吴云霞张明明韩涛冯旭高新陈静
Owner 淄博德丰化工有限公司
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