Epoxiconazole preparation method thereof

The technology of epoxiconazole and fluorobenzene is applied in the field of preparation and preparation of epoxiconazole, which can solve the problems of high environmental requirements for preparation of epoxiconazole, complicated preparation method of epoxiconazole, and failure of preparation, and achieves low cost and high cost. Stereoselective, step-by-step effects

Inactive Publication Date: 2018-11-06
ABA CHEM NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a preparation method of epoxiconazole, which has the advantages of simple preparation method, etc., and solves the complicated preparation method of the traditional epoxiconazole, and the requirements for the preparation environment of epoxiconazole Higher, users need to use complicated preparation equipment and a variety of fine materials when preparing epoxiconazole, users often need to concentrate and be careful when preparing epoxiconazole, and a momentary mistake will lead to preparation failure, and all previous efforts will be wasted , loss of a large amount of consumables, users are very troubled by this problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment one: a kind of preparation method of epoxiconazole comprises the following steps:

[0018] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene ethyl ketone;

[0019] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature is kept at 50°C for 12 hours t...

Embodiment 2

[0024] Embodiment two: a kind of preparation method of epoxiconazole comprises the following steps:

[0025] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene ethyl ketone;

[0026] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature is kept at 75°C for 12 hours. ...

Embodiment 3

[0031] Embodiment three: a kind of preparation method of epoxiconazole comprises the following steps:

[0032] 1) Add fluorobenzene and solvent into a glass reaction bottle with a stirrer and a condenser. The ratio of fluorobenzene to acetyl chloride is 1:15. Considering the toxicity and cost, choose dichloroethane as the solvent, and stir Add dichloroethane dropwise, control the reaction temperature, and wait for 5 hours to fully react in the glass reaction bottle. After the reaction is completed, hydrolyze with hydrochloric acid, steam distill off excess fluorobenzene, and solvent extraction precipitates to obtain p-fluorobenzene Ethyl ketone, purity 93.2%, yield 82.1%;

[0033] 2) Add o-chlorobenzyl phosphate and n-butanol solvent into a reaction flask with a stirrer and a condenser, continue heating from 0°C to 150°C, add p-fluoroacetophenone and o-chlorobenzyl phosphoric acid dropwise under stirring The ratio of ester to p-fluoroacetophenone is 1:2, and the temperature i...

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PUM

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Abstract

The invention relates to the technical field of chemical industry, and discloses an epoxiconazole preparation method. The method comprises the following steps: adding fluorobenzene and a solvent in aglass reaction bottle equipped with a stirrer and a condenser, wherein the ratio of fluorobenzene to acetyl chloride is 1:15, selecting dichloroethanes as the solvent by taking regard of toxicity andcost, dropping dichloroethanes under stirring, controlling the reaction temperature for fully reacting the materials in a glass reaction bottle after 5 hours, after the reaction is completed, performing hydrolysis with hydrochloric acid, steaming excessive fluorobenzene by water vapor, and performing desolvation through solvent extraction to obtain the fluoroacetophenone. The preparation method ofthe epoxiconazole is characterized in that a synthesis route is integrally improved, the preparation method has the advantages of simple process, and low cost and easy acquisition of raw material, the epoxiconazole has high stereoselective performance, cannot generate high salt waste water, does not use severe-toxicity methanesulfonyl chloride, accords with environmental protection requirement, and is suitable for industrial production, and the yield and content of the final product are high.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of epoxiconazole. Background technique [0002] At present, most of the fungicides used in my country's agricultural production are old varieties of organosulfur, organophosphorus and triazoles such as triadimefon and triadimenol. As a result, the pollution to the environment is becoming more and more serious. Epoxiconazole is a new generation of triazole fungicides with high activity and broad spectrum, which has special effects on target diseases. [0003] The traditional preparation method of epoxiconazole is relatively complicated, and the requirements for the preparation environment of epoxiconazole are relatively high. When preparing epoxiconazole, users need to use complicated preparation equipment and various fine materials. Epoxiconazole often needs to concentrate and be careful, and a momentary mistake will lead to preparation failure, all...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/06
CPCC07D405/06
Inventor 蒋信义徐军刘汝章
Owner ABA CHEM NANTONG
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