Method for synthesizing 2,5-acetonyl acetone

A synthesis method, the technology of hexanedione, which is applied in the field of organic compound synthesis, can solve problems such as environmental pollution, and achieve the effects of cost reduction, purity improvement, and mild reaction conditions

Inactive Publication Date: 2009-05-06
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although this method is simple and the yield is relatively high, a large amount of acetic acid and catalyst sulfuric acid will be used in the reaction, and a large am

Method used

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  • Method for synthesizing 2,5-acetonyl acetone
  • Method for synthesizing 2,5-acetonyl acetone
  • Method for synthesizing 2,5-acetonyl acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A method for synthesizing 2,5-hexanedione, the reaction scheme is

[0051]

[0052] Follow the steps in the following order:

[0053] a. Preparation of 2,5-hexanedione

[0054] Add 1000g of raw material 2,5-dimethylfuran into the four-neck flask, add 400g of glacial acetic acid, 480g of water, and 30mL of 10% sulfuric acid, reflux at 82°C for 48 hours, take a sample and extract it with ethyl acetate, and detect it by gas chromatography. The raw material content is 1.5% (less than 2%), and the temperature is lowered to obtain the reaction solution A; wherein the gas chromatography detection condition is:

[0055] Chromatographic column: SE-30 capillary column, 30m×0.25mm×0.25μm

[0056] Column temperature: 110°C / 5min—>20°C / min—>260°C / 5min;

[0057] Vaporization chamber temperature: 260°C; detection chamber temperature: 260°C;

[0058] Carrier gas pressure (N 2 ): 80kpa; Injection volume: 0.2μL;

[0059] Quantitative method: peak area normalization method; split ...

Embodiment 2

[0070] A method for synthesizing 2,5-hexanedione, the reaction scheme is

[0071]

[0072] Follow the steps in the following order:

[0073] a. Preparation of 2,5-hexanedione

[0074] Add the 10% sulfuric acid of raw material 2,5-dimethylfuran 990g, glacial acetic acid 170g, water 120g, 30mL in the four-necked bottle, and add the gained F10g of embodiment 1, G411g (containing 82g acetic acid, 328g water) and 180g D ( Containing 148g acetic acid, 32g water), refluxed at 82 ℃ for 48 hours, extracted with ethyl acetate after sampling, then utilized the same gas chromatography as Example 1 to detect the raw material content, the measured result was 1.7% (less than 2%), The temperature was lowered to obtain the reaction solution A.

[0075] b. Removal of the previous fraction

[0076] Add 9 g of sodium acetate to the reaction solution A, and stir at room temperature for 30 minutes. Atmospheric distillation to remove 410g of fraction B before 110°C, then add 120g of water to ...

Embodiment 3-6

[0083] The difference between Embodiment 3-6 and Embodiment 1 lies in the difference in the amount of substances used and the different reaction conditions, which can refer to the above table. Of course, corresponding data such as the amount of reaction product, the raw material content measured before cooling in step a, chromatogram, product yield and purity, acetic acid content in G and D must be different because of the above data differences (not shown in the table) out).

[0084] In their synthetic method steps, the remaining contents are consistent.

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Abstract

The invention discloses a method for synthesizing 2, 5-hexanedione, which comprises the steps of the preparation of the 2, 5-hexanedione, the removal of front cut fraction, the refining of the 2, 5-hexanedione and so on. 2,5-dimethylfuran is taken as a raw material to synthesize the 2, 5-hexanedione, a step of adding water for atmospheric distillation after the removal of the front cut fraction is added during the synthesis, so the difficulty of the separation when a product is subjected to vacuum rectification is reduced, and the purity of the product is greatly improved; the front cut fraction and a transitional distillate can further be circularly used for the feeding during the post-synthesis so as to further improve the yield (can reach up to more than 90 percent), reduce the cost for the whole synthetic route, and has no pollution to the environment. The method has simple needed equipment, mild reaction conditions, and safe and easy operation, is suitable for industrialized production, is a more reasonable and more convenient novel way for circularly and economically synthesizing the 2, 5-hexanedione, and can prepare an intermediate, namely the 2, 5-hexanedione which is widely applied in fields such as medicine, spices, pesticides, photographic reagents, electroplating and paint-spraying.

Description

technical field [0001] The invention belongs to the field of organic compound synthesis, and relates to a preparation method of a compound widely used in the fields of medicine, fragrance, insecticide, photographic agent, electroplating spray paint, etc., specifically a method for synthesizing 2,5-hexanedione Methods. Background technique [0002] 2,5-Hexanedione is an important organic chemical intermediate, which is widely used in the fields of medicine, spices, pesticides, photographic agents, electroplating and spray paint, etc. There are many synthetic methods of 2,5-hexanedione, and the ones reported using 2,5-dimethylfuran as raw materials include the following: [0003] ① Shenk et al. used 2,5-dimethylfuran to oxidize and open the ring to obtain 3-ene-2,5-hexanedione, and then hydrogenated and reduced it to obtain 2,5-hexanedione. The reaction route is as follows: [0004] [0005] In this method, the operation and control of hydrogenation reaction is difficult,...

Claims

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Application Information

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IPC IPC(8): C07C49/12C07C45/62C07C45/37
Inventor 张越魏爽
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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