Synthesis method of 2, 4-dichloroacetophenone

A kind of technology of dichloroacetophenone and synthetic method, applied in 2 fields, can solve the problems such as insufficient effect, waste of resources, high catalyst usage, etc., to achieve improved yield and purity, improved utilization rate, and improved utilization of raw materials rate effect

Inactive Publication Date: 2021-03-16
JIANGXI YONGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some enterprises have made great improvements in equipment and the use of rectification towers can achieve a certain increase in selectivity and yield, but the effect is still not obvious enough, and the amount of catalyst used remains high, which not only wastes resources, And it brings huge pressure on the cost control of industrialized production

Method used

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  • Synthesis method of 2, 4-dichloroacetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of synthetic method of 2,4-dichloroacetophenone, comprises the following content:

[0025] The raw materials include 62 parts by weight of m-dichlorobenzene, 33 parts of acetyl chloride, 30 parts of catalyst, and 25 parts of water; the specific method is:

[0026] (1) Add m-dichlorobenzene into the reaction tank, raise the temperature to 45°C at 2°C / min, add 40% of the catalyst by weight at 180rpm, keep the temperature constant for 30min, keep the speed constant, and then add 30% The above parts by weight of the catalyst, then add the above parts by weight of acetyl chloride dropwise within 1 hour, raise the temperature to 65°C, keep the temperature for 15 minutes, add the remaining catalyst by weight above, raise the temperature to 95°C at 3°C / min, and stir the reaction at this temperature 7h, stirring speed is 420rpm;

[0027] (2) Keep the stirring rate constant, cool down to 60°C naturally, add 5 parts of modified molecular sieve catalyst, react at constant t...

Embodiment 2

[0037] A kind of synthetic method of 2,4-dichloroacetophenone, comprises the following content:

[0038] The raw materials include 95 parts of m-dichlorobenzene, 62 parts of acetyl chloride, 50 parts of catalyst and 45 parts of water in parts by weight; the specific method is:

[0039] (1) Add m-dichlorobenzene into the reaction tank, raise the temperature to 55°C at 5°C / min, add 40% of the catalyst by weight at a speed of 300rpm, keep the temperature constant for 60min, keep the speed constant, and then add 30% The above weight parts of catalyst, then dropwise add the above weight parts of acetyl chloride within 2 hours, raise the temperature to 75 ° C, keep the temperature for 30 min, add the remaining above weight parts of catalyst, raise the temperature to 115 ° C at 7 ° C / min, and stir the reaction at this temperature 10h, stirring speed is 650rpm;

[0040] (2) Keep the stirring rate constant, cool down to 70°C naturally, add 15 parts of modified molecular sieve cataly...

Embodiment 3

[0050] A kind of synthetic method of 2,4-dichloroacetophenone, comprises the following content:

[0051] The raw materials include 78 parts of m-dichlorobenzene, 48 parts of acetyl chloride, 40 parts of catalyst and 35 parts of water in parts by weight; the specific method is:

[0052] (1) Add m-dichlorobenzene into the reaction tank, raise the temperature to 50°C at 3°C / min, add 40% of the catalyst by weight at 240rpm, keep the temperature constant for 45min, and then add 30% The above parts by weight of the catalyst, then add the above parts by weight of acetyl chloride dropwise within 1.5 hours, raise the temperature to 70°C, keep the temperature constant for 22min, add the remaining catalyst by weight above, raise the temperature to 105°C at 5°C / min, and stir at this temperature Reaction 8h, stirring speed is 550rpm;

[0053] (2) Keep the stirring rate constant, lower the temperature to 65°C naturally, add 10 parts of modified molecular sieve catalyst, react at constant t...

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Abstract

The invention provides a synthesis method of 2, 4-dichloroacetophenone, which breaks through a conventional temperature curve, effectively enhances the utilization ratio of the catalyst by using temperature change and adding the catalyst in different time periods according to the proportion, and promotes the reaction degree to be more thorough. Meanwhile, a modified mixture of aluminum chloride and ferric chloride is adopted as the catalyst, and the catalyst is supported on the porous support by utilizing the porous support, so that the activity of the catalyst is improved, the yield and the purity are improved, and the reaction rate and the reaction degree are prevented from being reduced due to catalyst deposition in the reaction process; and besides, in the reaction process, the modified molecular sieve catalyst is used for carrying out directional isomerization treatment on the by-product, the treated modified molecular sieve catalyst has high stability and high selectivity, the p-dichlorobenzene by-product and the o-dichlorobenzene by-product in the reaction process are converted into the reaction raw material m-dichlorobenzene, the utilization rate of the raw material is increased, and the generation of the by-product is reduced.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a synthesis method of 2,4-dichloroacetophenone. Background technique [0002] 2,4-Dichloroacetophenone is an important fine chemical intermediate, which is widely used in the fields of medicine and pesticides; for example, 2,4-Dichloroacetophenone can be used to synthesize the anti-deep fungal infection drug Flucan azole and itraconazole; can also synthesize low-toxic, broad-spectrum, systemic fungicides teconazole, metroconazole, etoconazole, propiconazole. At present, most of the synthesis of 2,4-dichloroacetophenone is based on m-dichlorobenzene and acetyl chloride or acetic anhydride as raw materials, and the acetylation reaction is carried out under the catalysis of Lewis acid aluminum chloride to obtain 2,4-dichloroacetophenone. Acetophenone. Although some enterprises have made great improvements in equipment and the use of rectification towers can ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/807C07C45/46B01J29/072B01J29/40
CPCC07C45/46B01J29/072B01J29/40B01J35/0006B01J2229/186B01J2229/20C07C49/807
Inventor 刘忠春
Owner JIANGXI YONGTONG TECH
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