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A kind of synthetic method of cracking and preparing cyclopropyl methyl ketone

A technology of cyclopropylmethyl ketone and its synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of strong corrosion, high cost, and low product yield, and achieve High selectivity, avoiding three wastes and high activity

Active Publication Date: 2021-07-13
JIANGSU YUXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 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 synthetic method of cracking and preparing cyclopropyl methyl ketone
  • A kind of synthetic method of cracking and preparing cyclopropyl methyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) In the jacketed reactor, add 200 g of solvent dimethyl sulfoxide, add 10 g of catalyst (sodium chloride: ZIF-67=1:0.1), start stirring, start heating, and raise the temperature to 100 ° C;

[0026] 2) At a temperature of 100°C, α-acetyl-γ-butyrolactone is slowly and continuously added to cause a catalytic cracking reaction, and at the same time, the cracking product cyclopropyl methyl ketone is continuously extracted through a rectification tower.

[0027] 3) After the raw material feeding is completed, continue to distill and extract for 2 hours, and collect the complete product cyclopropyl methyl ketone. After the reaction, the obtained solvent and catalyst can be directly used for the preparation of the next batch of cyclopropyl methyl ketone products without any treatment.

[0028] The collected cyclopropyl methyl ketone has a purity of 99.0%, and the total molar yield of the reaction is 98.1%.

Embodiment 2

[0030] 1) In the jacketed reactor, add 200 g of solvent N,N-dimethylformamide, add 50 g of catalyst (sodium iodide: ZIF-67=1:0.5), start stirring, start heating, and raise the temperature to 140°C;

[0031] 2) At a temperature of 140°C, α-acetyl-γ-butyrolactone is slowly and continuously added to cause a catalytic cracking reaction, and at the same time, the cracking product cyclopropyl methyl ketone is continuously extracted through the rectification tower.

[0032] 3) After the raw material feeding is completed, continue to distill and extract for 1 hour, and collect the complete product cyclopropyl methyl ketone. After the reaction, the obtained solvent and catalyst can be directly used for the preparation of the next batch of cyclopropyl methyl ketone products without any treatment.

[0033] The collected cyclopropyl methyl ketone has a purity of 99.8%, and the total molar yield of the reaction is 99.7%.

Embodiment 3

[0035] 1) In the jacketed reactor, add solvent chlorobenzene 200g, add catalyst 20g (potassium iodide: ZIF-67=1:0.2), start stirring, start heating, and raise the temperature to 110°C;

[0036] 2) At a temperature of 110°C, α-acetyl-γ-butyrolactone is slowly and continuously added to cause a catalytic cracking reaction, and at the same time, the cracking product cyclopropyl methyl ketone is continuously extracted through the rectification tower.

[0037] 3) After the raw material feeding is completed, continue to distill and extract for 2 hours, and collect the complete product cyclopropyl methyl ketone. After the reaction, the obtained solvent and catalyst can be directly used for the preparation of the next batch of cyclopropyl methyl ketone products without any treatment.

[0038] The collected cyclopropyl methyl ketone has a purity of 99.3%, and the total molar yield of the reaction is 98.5%.

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Abstract

The invention discloses a synthesis method for preparing cyclopropyl methyl ketone by cracking, which comprises adding a solvent and a catalyst in a jacketed reactor, starting stirring, starting heating, and raising the temperature to 100-140°C; at 100-140°C Under the temperature, slowly and continuously add α-acetyl-γ-butyrolactone, a catalytic cracking reaction occurs, and at the same time continuously extract the cracking product cyclopropyl methyl ketone through the rectification tower and other steps. The combined catalyst adopted in the invention has high catalytic efficiency, high activity and high selectivity, which not only reduces the reaction temperature, but also reduces other side reactions of cracking at high temperature, reduces energy consumption and costs at the same time. The raw material α-acetyl-γ-butyrolactone is catalyzed and cracked by this catalytic system, and the reaction has a high degree of selectivity under the stated conditions, and the reaction is almost free of impurities. During the reaction, the generation of three wastes is completely avoided, and the environment is protected; Dangers that may occur during high-temperature production are safer and help to improve operational efficiency.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a synthesis method for preparing cyclopropyl methyl ketone by cracking. Background technique [0002] Cyclopropyl methyl ketone 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] Cyclopropylmethyl ketone is a transparent liquid, and there are many ways to synthesize it, 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 me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/54C07C45/82C07C49/293
CPCC07C45/54C07C45/82C07C2601/02C07C49/293
Inventor 张治国徐官根徐林斌黄剑程红伟
Owner JIANGSU YUXIANG CHEM
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