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A kind of preparation method of 2,4-dichlorobenzonitrile

A technology of dichlorobenzonitrile and dichlorobenzyl alcohol, which is applied in the field of preparation of 2,4-dichlorobenzonitrile, can solve the problems of high comprehensive cost, reduce production cost, improve product quality, and avoid the use of metal catalysts Effect

Active Publication Date: 2020-06-05
河南省洛阳水文水资源勘测局
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of preparation method of 2,4-dichlorobenzonitrile in order to solve the deficiency of above-mentioned technical problem, overcome the problem that the comprehensive cost such as using metal catalyst or dangerous reaction reagent etc. is high in the existing method

Method used

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  • A kind of preparation method of 2,4-dichlorobenzonitrile

Examples

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Effect test

Embodiment 1

[0019] Add magneton, 2mL glacial acetic acid, 0.5mmol 2,4-dichlorobenzyl alcohol, 1.5mmol ammonium acetate, 0.15mmol nitric acid and 0.15mmol tetramethylpiperidine nitrogen oxide into the glass reaction tube in sequence (the pressure of oxygen is 1atm ). After the reaction test tube was sealed, it was put into a heating tank at 50° C., and reacted for 12 hours under magnetic stirring. Once the reaction time was reached, the reaction system was cooled to room temperature, and the product was subjected to internal standard quantitative analysis by gas chromatography, and the yield of 2,4-dichlorobenzonitrile product was obtained as 93%. Then the above experiment was repeated, and the product was separated and purified by column chromatography to obtain 2,4-dichlorobenzonitrile product. use 1 H-NMR, 13 C-NMR confirmed the product structure see figure 1 and 2 .

Embodiment 2

[0021] Add magnetite, 2 mL of glacial acetic acid, 0.5 mmol of 2,4-dichlorobenzyl alcohol, 1.5 mmol of ammonium acetate, 0.15 mmol of nitric acid, and 0.15 mmol of tetramethylpiperidine nitroxide into a glass-lined autoclave in sequence. After the reaction kettle was sealed, it was filled with 10atm oxygen, placed in a heating tank at 50°C, and reacted for 12 hours under magnetic stirring. Once the reaction time was reached, the reaction system was cooled to room temperature, and the internal standard quantitative analysis of the product was carried out by gas chromatography, and the yield of 2,4-dichlorobenzonitrile product was obtained as 77%.

Embodiment 3-4

[0023] The ammonium acetate in Example 1 was changed to ammonium sulfate and ammonium nitrate, and other conditions were unchanged, so that the yield of the product (gas-phase internal standard) was 63%, 52%, respectively.

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Abstract

The invention relates to a preparation method of 2,4-dichlorobenzonitrile. 2,4-dichlorbenzyl alcohol and a nitrogen source are dissolved in glacial acetic acid; oxygen gas is introduced; a mixture ofnitric acid and tetramethylpiperidine oxynitride is added as a catalyst; reaction is performed for 1 to 24h at the temperature of 25 to 100 DEG C in a sealed reactor; 2,4-dichlorobenzonitrile is obtained. The preparation method has the advantages that nonmetal is used as the catalyst; the oxygen gas is used as an oxidizing agent; the use of a metallic catalyst is avoided; the environment pollutionis reduced.

Description

technical field [0001] The invention relates to the technical field of chemical raw material preparation, in particular to a preparation method of 2,4-dichlorobenzonitrile. Background technique [0002] 2,4-Dichlorobenzonitrile is a widely used pesticide intermediate, which can be used in the production of fluorine-containing benzoylurea insecticides, herbicides, and water quality analysis reagents. It is also used in plastics, dyes, and electronic materials. Must apply. At present, there are many synthetic methods for dihalogenated benzonitriles, among which the ammoxidation method is relatively common. The raw material used is 2,4-dichlorobenzylbenzene, and VPO composite oxides are used as catalysts to react with ammonia under the oxidation of oxygen. The reaction produces 2,4-dichlorobenzonitrile. This method has a short route and low cost of raw materials; however, it is difficult to develop a stable catalyst and requires high production equipment. In addition, 2,4-di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/00C07C255/50
CPCC07C253/00C07C255/50
Inventor 程卫习鲍瑞雪范思源刘迎郑艺樊洪波谷彦彬郝亚楠赵荣荣王晓君王颖颖魏克明王福程宇洁薛沛
Owner 河南省洛阳水文水资源勘测局
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