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Method for preparing 2,4-dichloroacetophenone

A technology of dichloroacetophenone and m-dichlorobenzene, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, which can solve the problems of low preparation yield and poor purity, and achieve simple synthesis process , Promote dissolution and reduce reaction time

Pending Publication Date: 2021-11-09
NINGXIA RUITAI TECH +1
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Problems solved by technology

[0005] The application provides a method for preparing 2,4-dichloroacetophenone, which solves the problems of low yield and poor purity of 2,4-dichloroacetophenone in the prior art

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  • Method for preparing 2,4-dichloroacetophenone
  • Method for preparing 2,4-dichloroacetophenone

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Embodiment Construction

[0022] In order to enable those skilled in the art to better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the accompanying drawings.

[0023] see Figure 1-2

[0024] Known by above technical scheme, 1, a kind of method for preparing 2,4-dichloroacetophenone comprises the following steps:

[0025] S1: Mix and stir dichlorobenzene, aluminum trichloride, and amide additives;

[0026] S2: When the stirring temperature rises to 40°C, add acetyl bromide dropwise to it for reaction, the dropwise addition process lasts for 2-3 hours and keep warm for 1-2 hours after the temperature is raised to 100°C, and when the temperature is lowered to 50°C, 2,4-dichloroacetophenone synthetic liquid;

[0027] S3: Add the 2,4-dichloroacetophenone synthesis liquid in step 2 to hydrochloric acid for acidolysis and layering, and separate the oil...

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Abstract

The invention discloses a method for preparing 2,4-dichloroacetophenone. The method comprises the following steps: S1, weighing dichlorobenzene, aluminum trichloride and an amide auxiliary agent, and carrying out mixing and stirring; S2, when a stirring temperature rises to 40 DEG C, dropwise adding acetyl bromide for a reaction so as to obtain 2, 4-dichloroacetophenone synthetic liquid; S3, adding the 2,4-dichloroacetophenone synthetic liquid obtained in the step 2 into hydrochloric acid for acidolysis layering, and separating and washing an oil layer after layering; S4, dehydrating the washed oil layer in a vacuum environment system, and removing light components when the temperature rises to 98 DEG C; and S5, rectifying the residues after dehydration and light component removal to obtain the 2,4-dichloroacetophenone. According to the invention, acetyl bromide is adopted as a raw material, so the activity of an electrophilic reagent can be effectively reduced, and the yield of the product can be further improved. Meanwhile, the amide auxiliary agent is supplemented in the preparation process of the 2,4-dichloroacetophenone synthetic liquid, so the dissolution of aluminum trichloride is promoted, a contact area of reactants is increased, and reaction efficiency is greatly improved.

Description

technical field [0001] The application relates to the field of fine chemicals, in particular to a method for preparing 2,4-dichloroacetophenone. Background technique [0002] 2,4-Dichloroacetophenone is an important pesticide and pharmaceutical intermediate, mainly used in the synthesis of difenoconazole, ketoconazole and other fungicides. [0003] In 2008, Wang Yazhen of Jiangsu Technical Normal University published an article entitled "Research on the Synthesis Process of 2,4-Dichloroacetophenone" in "Chemical Engineer". The article used m-dichlorobenzene, acetic anhydride and trichloride Aluminum is used as a raw material, and 2,4-dichloroacetophenone is obtained through the processes of synthesis, hydrolysis, extraction, washing, light removal and rectification, with a yield of 81.8%. The process uses acetic anhydride, which is prone to poisonous production, as a raw material, and the steps are cumbersome and the yield is low. [0004] In 2021, Jiangxi Yongtong Technol...

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Application Information

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IPC IPC(8): C07C49/807C07C45/45C07C45/82
CPCC07C45/455C07C45/82C07C49/807
Inventor 朱斌刘勇石苏洋党大徽李梅马西宝亢玉荣马荣慧
Owner NINGXIA RUITAI TECH
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