Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for synthesizing chlorantraniliprole

A technology for chlorantraniliprole and benzamide, which is applied in the field of chlorantraniliprole synthesis, can solve the problems of high difficulty in industrialization, high requirements for synthesis steps, single method for synthesizing chlorantraniliprole, and the like, and achieves post-processing Simple, easy-to-use effects

Inactive Publication Date: 2021-10-08
江西汇和化工有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the common synthesis method of chlorantraniliprole is relatively single, and the overall synthesis steps require high requirements. Reaction environments such as high vacuum, high refrigeration, high temperature, fire and pressure are often used, and different equipment is required for processing, which is difficult to industrialize.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;

[0026] S2. Dissolve N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, keep stirring for 5 minutes, and add dropwise hydrogen peroxide with a mass concentration of 30%. , temperature controlled at 12°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;

[0027] S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 3 hours, get 3-amino-5-methylpyrazole, to 3-amino Adjust the pH value to 2 during the stirring process of crotononitrile and hydrazine hydrate, and stir in i...

Embodiment 2

[0033] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;

[0034] S2, dissolving N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, stirring continuously for 10 minutes, and adding hydrogen peroxide with a mass concentration of 30% dropwise , temperature controlled at 28°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;

[0035] S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 4 hours, get 3-amino-5-methylpyrazole, to 3-amino During the stirring process of crotononitrile and hydrazine hydrate, adjust the pH value to 3,...

Embodiment 3

[0041] S1. Stir the solvent containing 2-amino-3-methylbenzoic acid, wherein the solvent is an ether compound, and dropwise add methylamine solution during the stirring reaction process, heat to reflux, then extract and dry to obtain N- Methyl-3-methyl-2-amino-benzamide;

[0042] S2. Dissolve N-methyl-3-methyl-2-amino-benzamide in lye, wherein the lye is an aqueous solution of potassium tert-butoxide, keep stirring for 8 minutes, and add dropwise hydrogen peroxide with a mass concentration of 30%. , temperature controlled at 25°C, after the reaction, carry out halogenation reaction with NCS to obtain N-methyl-3-methyl-2-amino-5-chloro-benzamide;

[0043]S3, select 3-aminocrotononitrile to stir, add hydrazine hydrate to mix during stirring, carry out ring closing reaction, rise to room temperature naturally and react for 4 hours, get 3-amino-5-methylpyrazole, to 3-amino During the stirring process of crotononitrile and hydrazine hydrate, adjust the pH value to 3, and stir in i...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for synthesizing chlorantraniliprole, which comprises the following steps: stirring a solvent containing 2-amino-3-methyl benzoic acid, dropwise adding a methylamine solution in the stirring reaction process, dissolving N-methyl-3-methyl-2-amino-benzamide in an alkali liquor, carrying out a halogenation reaction with NCS(N-Chlorantraniliprole) after the reaction is finished, obtaining N-methyl-3-amino-5-chlorantraniliprole, performing a subsequent ring closing reaction, a bromination reaction, an oxidation reaction and a condensation reaction, an amidation reaction through cooperation of a catalyst, and obtaining chlorantraniliprole. According to the method, the preparation steps of chlorantraniliprole are optimized, the whole technological process is more in steps but simple in post-treatment, an intermediate product can be directly obtained after a single step is finished, high environmental control requirements are not needed in the whole synthesis steps, and industrialization can be conveniently achieved.

Description

technical field [0001] The invention belongs to the technical field of chlorantraniliprole synthesis, and more specifically relates to a method for synthesizing chlorantraniliprole. Background technique [0002] Chlorantraniliprole is a broad-spectrum insecticide with a new structure. It can also control various non-lepidopteran pests such as Coleoptera Weevilidae, Chrysoplastidae, Diptera Liminidae, and Bemisia tabaci. [0003] At present, the common synthesis method of chlorantraniliprole is relatively simple, and the overall synthesis steps require high requirements. Reaction environments such as high vacuum, high refrigeration, high temperature and high pressure are often used, and different equipment is required for processing, which makes industrialization difficult. Contents of the invention [0004] The purpose of the present invention is to solve the shortcomings existing in the prior art. By optimizing the preparation steps of chlorantraniliprole, the whole proc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 李辉虎孙国强姜永亮谢林涛
Owner 江西汇和化工有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products