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Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound

A technology of dicarbonyl compounds and synthesis methods, which is applied in the field of synthesis of β-chlorinated α, γ-dicarbonyl compounds, can solve problems such as high reaction cost, low yield, low purity, and environmental pollution, and achieve reduction of side reactions, Simple post-processing, the effect of improving the conversion rate

Active Publication Date: 2021-03-30
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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  • Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound
  • Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound
  • Synthesis method of beta-chloro-alpha, gamma-dicarbonyl compound

Examples

Experimental program
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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 particularly discloses a synthesis method of a beta-chloro-alpha, gamma-dicarbonyl compound. The synthesis method comprises thefollowing steps: under a solvent-free condition, taking an alpha, gamma dicarbonyl compound shown as a formula (I) as a raw material, taking anhydrous aluminum chloride as a catalyst, and introducingchlorine to carry out chlorination reaction, so as to obtain the beta-chlorinated alpha, gamma dicarbonyl compound shown as a formula (II). The beta-chloro-alpha, gamma-dicarbonyl compound shown in the formula (II) is prepared through a chlorination reaction by taking chlorine as a chlorination reagent and taking anhydrous aluminum chloride as a catalyst under a solvent-free condition, a product with the purity of more than 90% can be obtained only through simple post-treatment of a reaction product, the yield can reach 90% or above. The method has the advantages of mild reaction conditions, simple process operation, no generation of sulfur dioxide polluting the environment, greenness, environmental protection, and suitableness 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 Applications(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
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