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A kind of new preparation method of cyclopropanone

A technology of cyclopropane ketone and methyl imidazolium ion is applied in the preparation of heterocyclic compounds, organic chemistry and other directions, which can solve the problems of low reaction yield, high reaction temperature and high cost, achieve high reaction selectivity and improve operation efficiency. , avoid dangerous effects

Active Publication Date: 2022-01-25
JIANGSU YUXIANG CHEM
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The reaction temperature of this route is too high, which is difficult for general enterprises to achieve. At the same time, the reaction yield is low, generally lower than 90%, and the product content is also low, containing more cracking by-products
[0005] There are more or less defects in the various existing synthetic methods, or the product yield is low, or the corrosion is too strong in the reaction process, or the cost is too high
Existing technical routes need to be improved in terms of environmental friendliness and cost

Method used

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  • A kind of new preparation method of cyclopropanone
  • A kind of new preparation method of cyclopropanone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) In the microwave reactor, add 200 g of 1-butyl-3-methylimidazolium chloride salt ionic liquid, start stirring, start microwave heating, and raise the temperature to 140°C;

[0024] 2) At a temperature of 140°C, slowly and continuously add α-acetyl-γ-butyrolactone, microwaves promote the catalyzed cracking reaction of the ionic liquid, and continuously extract the cracked product cyclopropanone through the rectification tower. The raw material addition rate was 10 g / min.

[0025] 3) After the raw material feeding is completed, the distillation is continued for 1 hour to collect the complete product cyclopropanone. After the reaction, the obtained ionic liquid can be directly used for the preparation of the next batch of cyclopropanone products without any treatment.

[0026] The content of the collected cyclopropanone was 99.10%, and the total molar yield of the reaction was 98.2%.

Embodiment 2

[0028] 1) In the microwave reactor, add 200 g of 1-ethyl-3-methylimidazolium bromide salt ionic liquid, start stirring, start microwave heating, and raise the temperature to 100°C;

[0029] 2) At a temperature of 100°C, α-acetyl-γ-butyrolactone is added slowly and continuously, microwaves promote the catalyzed cracking reaction of the ionic liquid, and at the same time, the cracked product cyclopropanone is continuously extracted through the rectification tower. The feed rate was 1.0 g / min.

[0030] 3) After the raw material feeding is completed, continue to distill and extract for 2 hours, and collect the complete product cyclopropanone. After the reaction, the obtained ionic liquid can be directly used for the preparation of the next batch of cyclopropanone products without any treatment.

[0031] The content of the collected cyclopropanone was 99.5%, and the total molar yield of the reaction was 98.9%.

Embodiment 3

[0033] 1) In the microwave reactor, add 200 g of 1-butyl-3-methylimidazolium iodide salt ionic liquid, start stirring, start microwave heating, and raise the temperature to 120°C;

[0034] 2) At a temperature of 120°C, α-acetyl-γ-butyrolactone is added slowly and continuously, microwaves promote the catalytic cracking reaction of the ionic liquid, and at the same time, the cracking product cyclopropanone is continuously extracted through the rectification tower. The feed rate was 2.0 g / min.

[0035] 3) After the raw material feeding is completed, the distillation is continued for 1 hour to collect the complete product cyclopropanone. After the reaction, the obtained ionic liquid can be directly used for the preparation of the next batch of cyclopropanone products without any treatment.

[0036] The content of the collected cyclopropanone was 99.70%, and the total molar yield of the reaction was 99.2%.

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Abstract

The invention discloses a new preparation method of cyclopropanone, which includes adding ionic liquid into a microwave reactor, starting stirring, starting microwave heating, and raising the temperature to 100-140°C; at a temperature of 100-140°C, slowly and continuously Add α-acetyl-γ-butyrolactone, microwave promotes the catalytic cracking reaction of ionic liquid, and continuously extract the cracking product cyclopropanone and other steps through the rectification tower. The present invention uses microwaves to promote the catalytic cracking of ionic liquid raw material α-acetyl- γ-butyrolactone, under the conditions, the reaction has a high selectivity, and the reaction is almost free of impurities. The cyclopropanone content of the product obtained by the method is greater than 99%, and the total reaction yield is greater than 98%, which is much higher than Traditional methods and literature reports. During the reaction process, the production of three wastes is completely avoided, which protects the environment; it avoids possible dangers in the high-temperature production process, which is safer and conducive to improving operational efficiency.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a new preparation method of cyclopropanone. Background technique [0002] Cyclopropanone, CAS number: 765-43-5, molecular formula: C5H8O. Cyclopropanone is an important organic raw material and intermediate. In medicine, it is mainly used in the synthesis of anti-AIDS drugs Efluverenz and Ilremin; in pesticides, it is mainly used in the synthesis of fungicides cyprodinil and cyproconazole. [0003] There are many ways to synthesize cyclopropanone, among which the raw material α-acetyl-γ-butyrolactone is more competitive. The raw material α-acetyl-γ-butyrolactone can undergo a hydrolysis halogenation reaction to generate a halogenated pentanone, and then undergo a ring closure reaction to obtain the product cyclopropanone. This route has too many wastes, serious pollution and high cost. [0004] U.S. Patent No. 5,254,739 discloses a new method. The raw ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/59C07C49/293
CPCC07C45/59C07C2601/02C07C49/293
Inventor 张治国徐官根徐林斌黄剑程红伟
Owner JIANGSU YUXIANG CHEM
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