Method for synthesizing 2,5-hexanedione by two-phase process

A technology of hexanedione and organic phase, which is applied in the field of hydrolysis to prepare 2,5-hexanedione, which can solve the problems of limited technology application, low yield, and many side reactions, and achieve the effect of improving catalytic efficiency

Active Publication Date: 2016-02-24
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned research has problems such as many side reactions, low yield and complicat

Method used

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  • Method for synthesizing 2,5-hexanedione by two-phase process
  • Method for synthesizing 2,5-hexanedione by two-phase process
  • Method for synthesizing 2,5-hexanedione by two-phase process

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Embodiment 1

[0027] Add 1ml of 2,5-dimethylfuran into the container, then add 10ml of methyl isobutyl ketone, 7ml of dilute sulfuric acid (9.8% by mass), and mix well. The container was placed in a constant temperature reactor at 120°C, and reacted for 24 hours. After the reaction, the container was put into an ice bath to quench the reaction, and the temperature of the system dropped rapidly to room temperature. The reaction product was taken out, the two phases were separated by centrifugation, and the organic phase was collected. The organic phase obtained is distilled under reduced pressure, removes organic solvent, obtains product (see attached image 3 with 4 ). The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography. The results showed that the conversion rate of the raw material 2,5-dimethylfuran was 97%, the purity of the product wa...

Embodiment 2

[0029] Into the container, sequentially add: 1ml 2,5-dimethylfuran, 10ml cyclohexane, 7ml dilute hydrochloric acid (mass fraction 3.7%), and mix evenly. The container was placed in a constant temperature reactor and reacted at 100° C. for 12 hours. After the reaction, the system was rapidly dropped to normal temperature. The reaction solution is centrifuged, and the obtained organic phase is distilled under reduced pressure to remove the organic solvent to obtain the product. The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography. The results showed that the conversion rate of the raw material 2,5-dimethylfuran was 89%, the purity of the product was 90%, and the yield of 2,5-hexanedione was 85%.

Embodiment 3

[0031] Add 1ml of 2,5-dimethylfuran into the container, then add 15ml of dichloromethane, 10ml of dilute phosphoric acid (mass fraction 8.5%), and mix well. The container was placed in a constant temperature reactor at 180°C, and reacted for 12 hours. After the reaction, the container was put into an ice bath to quench the reaction, and the temperature of the system dropped rapidly to room temperature. The reaction product is taken out, the aqueous phase and the organic phase are separated by centrifugation, the organic phase is collected, and the organic phase is subjected to vacuum distillation to remove the organic solvent to obtain the product. The conversion rate of the raw material and the yield of the product were determined by gas chromatography external standard method, and the purity of the product was determined by liquid chromatography. The results showed that the conversion rate of the raw material 2,5-dimethylfuran was 87%, the purity of the product was 92%, and...

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Abstract

The invention provides a method for synthesizing 2,5-hexanedione by a two-phase process, which comprises the steps of mixing 2,5-dimethylfuran with a weak-polarity organic solvent, adding an aqueous solution of an acid catalyst, quenching a reaction system, quickly cooling the system temperature to the room temperature, and taking the reaction liquid out, wherein the reaction temperature is 60 to 180 DEG C, and the reaction time is 30 minutes to 24 hours. An organic phase is split; an aqueous phase is filtered or separated through centrifugation; organic phases are collected. The obtained organic phases are subjected to reduced pressure distillation, and the organic solvent is removed so that the product 2,5-hexanedione is obtained. The method has the advantages of efficiency, economy, environment friendliness, and high yield.

Description

technical field [0001] The invention belongs to a method for preparing 2,5-hexanedione by hydrolyzing 2,5-dimethylfuran in a two-phase system. Background technique [0002] In recent years, 2,5-hexanedione has received more and more attention as an important chemical intermediate. 2,5-Hexanedione is often used as basic research in the fields of toxicology and neurobiology. It is also a metabolite of n-hexane and methyl n-butanone widely used in the chemical industry after being absorbed by the human body. Due to its special molecular structure, it is widely used in pharmaceutical raw materials, food additives, spices, photographic agents, synthetic resins, nitro spray paints, colorants, etc. It can also be used as a high boiling point solvent for printing inks, rubber vulcanization accelerators, There are huge applications in industry. [0003] There are many ways to synthesize 2,5-hexanedione. One way is to react ethyl acetoacetate sodium with pure iodine to generate diet...

Claims

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Application Information

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IPC IPC(8): C07C45/59C07C45/78C07C49/12
CPCC07C45/59C07C45/78C07C49/12
Inventor 杨永兴李岳秦邓天昇侯相林
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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