A kind of preparation method of imidacloprid

A technology of imidacloprid and chloromethylpyridinone, which is applied in the field of imidacloprid, can solve the problems of low yield of active ingredients and increased water content, and achieve the effect of reducing water content and increasing the content of active ingredients

Active Publication Date: 2022-06-17
江苏克胜集团股份有限公司
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the imidacloprid production process uses NaOH in the preparation process. Due to the strong hygroscopicity of NaOH, the moisture content increases during the production process. Moreover, using NaOH as the acid-binding agent, the hydroxide in NaOH will also react with the The reaction of the active groups in the raw materials will also lead to an increase in the water content in the reaction system, which will lead to the "hydroxylation" of the halogen atoms on the pyridine ring and the halogen atoms on the side chains in the raw materials and products due to hydrolysis, Ultimately lead to low yield of active ingredient in imidacloprid synthesis reaction

Method used

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  • A kind of preparation method of imidacloprid
  • A kind of preparation method of imidacloprid

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preparation example Construction

[0026] The invention provides a preparation method of imidacloprid, comprising the following steps:

[0027] Mixing 2-chloro-5-chloromethylpyridine butanone solution, butanone, phase transfer catalyst, imidazolidine and acid binding agent to obtain a mixed solution;

[0028] The mixed solution is subjected to a substitution reaction to obtain an initial reaction solution of imidacloprid;

[0029] The initial reaction solution of imidacloprid is sequentially desolvated and washed, and the organic phase is taken to obtain a purified reaction solution of imidacloprid, and the washing agent used in the washing includes water and butanone;

[0030] The imidacloprid purification reaction solution is crystallized to obtain the imidacloprid;

[0031] The acid binding agent includes one or more of trimethylamine, triethylamine and tripropylamine.

[0032] In the present invention, unless otherwise specified, all raw material components are commercially available products well known t...

Embodiment 1

[0057] Mix 100g butanone and 32.4g 2-chloro-5-chloromethylpyridine in a dropping funnel to prepare 132.4g 2-chloro-5-chloromethylpyridine butanone solution, in which 2-chloro-5-chloromethylpyridine The mass concentration of pyridine is 24.4%;

[0058] In the reaction flask, 200g of butanone, 0.5g of tetra-tert-butylammonium bromide, 31g of imidazolidine and 35.2g of trimethylamine were premixed at 65°C with stirring at a rate of 300r / min to obtain a premixed solution;

[0059] 132.4g of 2-chloro-5-chloromethylpyridine butanone solution was added dropwise to the premixed solution at a rate of 25g / h. During the dropwise addition, the pH value of the system was measured every 30min. , keep the pH value of the system at 8, and after the dropwise addition is completed, a mixed solution is obtained;

[0060] The mixed solution is subjected to a substitution reaction at 65° C. and a stirring rate of 300 r / min for 4 h to obtain an initial reaction solution of imidacloprid;

[0061] ...

Embodiment 2

[0066] Mix 100g butanone and 32.4g 2-chloro-5-chloromethylpyridine in a dropping funnel to prepare 132.4g 2-chloro-5-chloromethylpyridine butanone solution, in which 2-chloro-5-chloromethylpyridine The mass concentration of pyridine is 24.4%;

[0067] In the reaction flask, premix 220g butanone, 0.45g tetra-tert-butylammonium bromide, 30.5g imidazolidine and 20.2g triethylamine at 65°C with stirring at a rate of 300r / min to obtain a premixed solution ;

[0068] 132.4g of 2-chloro-5-chloromethylpyridine butanone solution was added dropwise to the premixed solution at a rate of 25g / h. During the dropwise addition, the pH value of the system was measured every 30min. Amine, keep the pH value of the system at 8, after the dropwise addition is completed, a mixed solution is obtained;

[0069] The mixed solution is subjected to a substitution reaction at 65° C. and a stirring rate of 300 r / min for 4 h to obtain an initial reaction solution of imidacloprid;

[0070] The initial re...

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Abstract

The invention relates to the technical field of imidacloprid synthesis, in particular to a preparation method of imidacloprid. In the preparation method provided by the invention, using one or more of trimethylamine, triethylamine and tripropylamine as the acid-binding agent can effectively reduce the hygroscopic effect of sodium hydroxide when sodium hydroxide is used as the acid-binding agent in the preparation process. The moisture brought to the preparation process effectively inhibits the hydrolysis side reaction of the reaction raw materials and products under the action of water during the reaction process, improves the active ingredients of the imidacloprid product, and at the same time reduces the moisture content of the product.

Description

technical field [0001] The invention relates to the technical field of imidacloprid, in particular to a preparation method of imidacloprid. Background technique [0002] Imidacloprid is a new variety of high-efficiency, systemic, and long-residual-effective agricultural pesticides. It is widely used in cotton, vegetables, fruit trees, rice, wheat and other crops to effectively control pests such as aphids, planthoppers, leafhoppers, and weevil . [0003] In the prior art, the imidacloprid production process uses NaOH in the preparation process. Due to the strong hygroscopicity of NaOH, the water content in the production process increases. Moreover, using NaOH as an acid binding agent, the hydroxide in the NaOH will also react with The reaction of the active groups in the raw materials will also lead to an increase in the moisture content in the reaction system, which will lead to the "hydroxylation" of the halogen atoms on the pyridine ring and the halogen atoms on the sid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/06
CPCC07D401/06
Inventor 吴静陆静
Owner 江苏克胜集团股份有限公司
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