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Catalytic synthesis method of propanil

A synthesis method, the technology of propanil, which is applied in the field of synthesis of propanil, achieves the effects of low production cost, simple process and simple post-treatment

Pending Publication Date: 2022-03-25
NINGXIA G R FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the elimination of iron ions is also a good way to block free radical reactions and improve the selective yield, and there are no relevant reports in this regard.

Method used

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  • Catalytic synthesis method of propanil
  • Catalytic synthesis method of propanil
  • Catalytic synthesis method of propanil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 164.42g of 3,4-dichloroaniline (purity 98.5%, 1mol), 133.23g of propionic anhydride, 0.16g of molecular sieve, 0.16g of phosphine / nitrogen compound into a 500mL four-neck flask, then slowly raise the temperature to 145-155°C, Reflux and keep warm for 3-4h. After the reaction, the generated propionic acid is distilled off, and then the molecular sieve is recovered by filtration, and then the remaining raffinate is cooled and stirred for crystallization, and then dried after the crystallization is complete to obtain the propanil product.

[0027] According to the above method, different molecular sieves and phosphine / nitrogen-containing compounds were used to synthesize propanil, and the results are shown in Table 1 below:

[0028] Table 1

[0029]

[0030]

[0031]

Embodiment 2

[0033] Add 164.39g 3,4-dichloroaniline (purity 98.5%, 1mol) in 500mL four-necked flask, 133.23g propionic anhydride, molecular sieve 5A of different quality, the phosphine / nitrogen compound of different quality (mass ratio 1:1 Cyclohexanediaminetetraacetic acid and benzyltriethylammonium chloride), slowly warm up to the reflux temperature of 145-155°C, and keep the reaction under reflux for 3-4h. After the reaction, the generated propionic acid is distilled off, and then the molecular sieve is recovered by filtration, and then the remaining raffinate is cooled and stirred for crystallization, and then dried after the crystallization is complete to obtain the propanil product.

[0034] The amount of molecular sieves and phosphine / nitrogen-containing compounds and the product situation are shown in Table 2 below:

[0035] Table 2

[0036]

[0037]

Embodiment 3

[0039] In a 500mL four-necked flask, add 164.39g 3,4-dichloroaniline (purity 98.5%, 1mol), different quality acylating agents, 0.16g molecular sieve 5A, 0.16g different phosphine / nitrogen compounds, slowly rise to Different temperature, insulation reaction 3-4h. After the reaction, the generated by-products are removed by distillation, and then the molecular sieves are recovered by filtration, and then the remaining raffinate is cooled and stirred for crystallization, and dried after the crystallization is complete to obtain the propanil product.

[0040] The situation of the propanil product obtained under different reaction conditions is shown in Table 3 below:

[0041] table 3

[0042]

[0043]

[0044] Note: The amount of acylating agent refers to the molar ratio of acylating agent to 3,4-dichloroaniline.

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Abstract

The invention discloses a catalytic synthesis method of propanil, which takes 3, 4-dichloroaniline as a main raw material, and comprises the step of reacting 3, 4-dichloroaniline with an acylating agent in the presence of a catalyst to synthesize propanil. By introducing the specific catalyst, the defects of low product content, poor yield and the like of the original process are effectively avoided, the reaction selectivity and the yield are obviously improved, and the method is suitable for industrial application.

Description

technical field [0001] The invention relates to a method for synthesizing propanil, in particular to a method for synthesizing propanil which uses a catalyst, has good reaction selectivity and high yield, and belongs to the technical field of propanil synthesis. Background technique [0002] Patents US3158650 and CN111320549 report the synthesis process of propanil, both of which use 3,4-dichloroaniline and propionic acid as raw materials and condense at high temperature to obtain the product. Under high temperature and strong acid conditions, the raw material 3,4-dichloroaniline is easy to generate benzoquinone and its polymers, which seriously affects the content and yield of the product. [0003] The thermal oxidation process of aniline compounds is a series of free radical reactions. Under the action of heat, light or oxygen, aniline undergoes free radical oxidation to generate benzoquinone and its polymers. It has been reported in the prior art that low-priced sulfur-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/15
CPCC07C231/02C07C233/15
Inventor 李志清迟志龙赵广理王济旋程元刚张国中杨知昆
Owner NINGXIA G R FINE CHEM CO LTD
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