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A kind of synthetic method of β-chloro α, γ-dicarbonyl compound

A technology for a dicarbonyl compound and a synthesis method, which is applied in the field of synthesis of β-chloro α,γ-dicarbonyl compounds, can solve the problems of environmental pollution, high reaction cost, low yield and purity, and achieves reduction of side reactions, Post-processing is simple and the effect of improving conversion rate

Active Publication Date: 2022-03-11
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of low yield, low purity, high reaction cost and environmental pollution in the synthesis method of β-chlorinated α,γ-dicarbonyl compounds in the prior art, the present invention provides a β-chlorinated α,γ-dicarbonyl compound Synthetic method of carbonyl compound

Method used

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  • A kind of synthetic method of β-chloro α, γ-dicarbonyl compound
  • A kind of synthetic method of β-chloro α, γ-dicarbonyl compound
  • A kind of synthetic method of β-chloro α, γ-dicarbonyl compound

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Effect test

Embodiment 1

[0031] A kind of synthetic method of 2-chloro-2-acetyl cyclopentanone:

[0032] Add 200g of 2-acetylcyclopentanone to a 1L four-necked bottle, put in an oil bath at 30°C, add 10.6g of anhydrous aluminum chloride, and feed chlorine gas under stirring conditions at a rate of 17g / h, and set tail gas absorption at the same time. After reacting for 7 hours, gas chromatography detected the completion of the reaction, washed twice with 50 mL of water, separated the liquid, and dried to obtain 254.9 g of crude 2-chloro-2-acetylcyclopentanone. The yield of the target product was 96%, and the gas chromatography purity was 96%.

Embodiment 2

[0034] A kind of synthetic method of 2-chloro-2-ethoxycarbonyl cyclopentanone:

[0035] Add 200g of 2-ethoxycarbonylcyclopentanone to a 1L four-neck flask, put in an oil bath at 30°C, add 8.5g of anhydrous aluminum chloride, and feed chlorine gas under stirring conditions at a feed rate of 11g / h, and set the tail gas absorption at the same time , reacted for 9h, gas chromatography detected the completion of the reaction, washed twice with 50mL of water, separated, and dried to obtain 232.9g of crude product of 2-chloro-2-ethoxycarbonylcyclopentanone. The yield of the target product was 93%, and the gas chromatography purity was 97%.

Embodiment 3

[0037] A kind of synthetic method of 2-chloro-2-acetylbutyrolactone:

[0038] Add 200g of 2-acetylbutyrolactone into a 500L four-necked bottle, put it in an oil bath at 40°C, add 30g of anhydrous aluminum chloride, and feed chlorine gas under stirring conditions at a rate of 30g / h. At the same time, set up tail gas absorption and react After 4 hours, the reaction was detected by gas chromatography, washed twice with 50 mL of water, separated, and dried to obtain 249.5 g of crude 2-chloro-2-acetylbutyrolactone. The yield of the target product was 92%, and the gas chromatography purity was 94%.

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Abstract

The invention relates to the technical field of chemical synthesis, and specifically discloses a synthesis method of β-chlorinated α, γ-dicarbonyl compounds. The synthesis method includes the following steps: under solvent-free conditions, using the α,γ-dicarbonyl compound represented by the formula (I) as a raw material, using anhydrous aluminum chloride as a catalyst, and introducing chlorine gas for chlorination reaction to obtain the formula β-chloro α,γ-dicarbonyl compounds shown in (II). In the present invention, under solvent-free conditions, chlorine gas is used as a chlorination reagent, anhydrous aluminum chloride is used as a catalyst, and under specific reaction conditions, the β-chlorinated α shown in formula (II) is prepared through a chlorination reaction. , γ-dicarbonyl compound, the reaction product can be obtained with a purity of more than 90% only after simple post-treatment, and the yield can reach more than 90%, the reaction conditions are mild, the process is easy to operate, and the reaction will not pollute the environment Sulfur dioxide, green and environmentally friendly, suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of β-chlorinated α, γ-dicarbonyl compounds. Background technique [0002] Organochlorine pesticides are organic compounds containing organochlorine in the components used to prevent and control plant diseases and insect pests. They are broad-spectrum insecticides with stable properties and good insecticidal effects. The broadest class of organic synthetic drugs. In recent years, new varieties of organochlorine pesticides have emerged continuously, therefore, this requires a variety of organochlorine compounds as raw materials. [0003] Chlorination reaction is a reaction that is widely used in industry to prepare organic chlorine compounds. Among them, the chlorination reaction of replacing hydrogen atoms is mostly, and the commonly used chlorination reagents are mainly hydrochloric acid, sulfuryl chloride and solid phosgene. In α,γ-dicarbonyl com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/28C07C49/457C07C49/463C07C69/757C07C67/307C07C45/63
CPCC07D307/28C07C45/63C07C67/307C07C2601/08C07C2601/14C07C49/457C07C49/463C07C69/757
Inventor 张博高永民李立华赵娜李志锋贾成国
Owner HEBEI VEYONG BIO CHEM