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Acylation reaction method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride

A technology of methylbutyryl chloride and acylation reaction, which is applied in chemical instruments and methods, carboxylate preparation, organic compound preparation, etc., can solve the problems of low quality and low reaction yield, and achieve stable reaction conditions, The effect of stable reaction conditions and increased yield

Inactive Publication Date: 2013-07-10
安徽海顺化工有限公司
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Problems solved by technology

The existing acylation process has problems such as low reaction yield and low quality

Method used

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Embodiment Construction

[0009] The acylation method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride comprises the following steps:

[0010] Add 930 kilograms of 2-4-(chlorophenyl)-3-methylbutyric acid, 10 kilograms of acetic acid, and 20 kilograms of activated carbon into the reactor, and add 510 kilograms of chlorinated oxychloride to the reactor at room temperature Sulfone, the reaction is an exothermic reaction, wait for the temperature to rise to 80°C, start stirring, after the addition of thionyl chloride is completed, keep it warm for 6 hours, filter out activated carbon and other impurities, and get 2-4-(Chlorophenyl)- 3-Methylbutyryl chloride crude product, the crude product is sucked into the distillation still with a vacuum pump to recover excess thionyl chloride, and the residue at the bottom of the still is 971 kg of 2-4-(chlorophenyl)-3-methylbutyryl chloride , The HCL and SO2 produced by the acylation reaction are absorbed by the falling film secondary stage to obtain a hydroc...

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Abstract

The invention discloses an acylation reaction method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride. The acylation reaction method comprises the following steps: adding 900-950 parts by weight of 2-4-(chlorophenyl)-3-methylbutyric acid, 10-12 parts by weight of acetic acid and 20-25 parts by weight of activated carbon into a reaction kettle, dripping 510-520 parts by weight of thionyl chloride into the reaction kettle at normal temperature, performing heat release reaction, increasing the temperature to 80 DEG C, then opening the reaction kettle, stirring, performing heat preservation for 6hours after the end of dripping of the thionyl chloride, and press-filtering out the activated carbon and other impurities to obtain a crude product 2-4-(chlorophenyl)-3-methylbutyryl chloride. According to the acylation reaction method, the activated carbon is adopted for heat absorption, so that the smooth reaction conditions can be ensured, the yield is greatly improved, the acetic acid is increased and the stable reaction conditions are ensured so as to be conductive to performing the reaction.

Description

technical field [0001] The invention relates to compound synthesis, in particular to an acylation reaction method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride. Background technique [0002] 2-4-(Chlorophenyl)-3-methylbutyryl chloride is an important fine chemical intermediate. Due to its continuous development and utilization in recent years, many downstream products have high added value. Domestic research started relatively late, and currently it is mainly used as a pesticide intermediate for the production of pyrethroid insecticides such as fenvalerate and lyfelin (proposed, that is, artificially imitated and chemically synthesized biological pesticides). [0003] The 2-4-(chlorophenyl)-3-methylbutyryl chloride production unit mainly includes: alkylation, hydrolysis, neutralization separation, acidification separation, acylation and other processes. The existing acylation process has problems such as low reaction yield and low quality. Contents of the inve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/76C07C51/60
Inventor 孙火青
Owner 安徽海顺化工有限公司
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