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Pymetrozine preparation method

A technology of pymetrozine and time control, applied in the direction of organic chemistry, etc., can solve the problems affecting product purity, low content of pymetrozine products, affecting product purity and yield, etc., so as to improve the conversion rate of raw materials and facilitate industrialized large-scale production , The effect of increasing product yield

Inactive Publication Date: 2015-08-19
ANHUI YANGZI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] 1. The aminotriazone hydrochloride produced in the acid hydrolysis process is relatively stable, while the free aminotriazone hydrochloride produced after neutralization is relatively active, and is easily hydrolyzed in neutral or weakly alkaline aqueous solution or oxidized in the air. Side reactions, the purity of the final pymetrozine product is generally around 95%, which affects the purity and yield of the product
[0015] 2. In the method of first neutralization and then condensation, the acid-base neutralization reaction is carried out first, which produces more salt. After neutralization, during the reaction with the nicotinic aldehyde solution, a large amount of salt is wrapped in the precipitated pymetrozine product, resulting in The content of pymetrozine product is low, which affects the purity of the product

Method used

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Experimental program
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Effect test

Embodiment 1

[0037] In the 1000mL reaction flask, install a stirrer, a thermometer, a constant pressure dropping funnel and a condenser. Add 500ml of pure water at room temperature, start stirring, add 100.0g of acetamidotriazone, and dropwise add 99.0g of 31% hydrochloric acid; heat up to 30-60°C and keep it warm for 3.0-10.0 hours. After the sampling analysis is qualified, cool down appropriately. Add 295g of nicotine aldehyde solution dropwise at 30°C-90°C for 1.5 hours. After the dropwise addition, keep the temperature for 1.0 hour and cool down appropriately. Slowly add about 105.5g of 17% ammonia water dropwise at 30°C-90°C. Add time for 1.0 hours, control neutralization end point pH=7.0, test with precision test paper, retest pH unchanged in 10 minutes; after neutralization is qualified, then heat up to 50°C-90°C and keep it warm for 3.0-8.0 hours, then cool Cooling and crystallization, suction filtration, washing with 100ml of water, the wet product of pymetrozine obtained was drie...

Embodiment 2

[0039] In the 1000mL reaction flask, install a stirrer, a thermometer, a constant pressure dropping funnel and a condenser. Add 500ml of methanol at room temperature, start stirring, add 100.0g of acetamidotriazone, and dropwise add 110.0g of 31% hydrochloric acid; heat up to 30-60°C and keep it warm for 3.0-8.0 hours. solvent, then lower the temperature properly, add 310g of nicotinic aldehyde solution dropwise at 30°C-90°C, and the dropping time is about 2.0 hours. The pH of the neutralization end point is about 7.5, and it is tested with precision test paper, and the pH remains unchanged after 10 minutes of retesting; after the neutralization is qualified, then heat up to 50°C-90°C and keep the temperature for 3.0-8.0 hours, then cool down to crystallize, and the suction filtration is smooth , washed with 150ml of water, and the wet product of pymetrozine obtained was dried with hot air at 100° C. to obtain a white pymetrozine product. The purity of the product was 98.0% th...

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Abstract

The invention discloses a pymetrozine preparation method. The method comprises that acetaminotriazone and an acid as raw materials undergo an acidolysis reaction to produce aminotriazone acid salt, the aminotriazone acid salt and a nicotinaldehyde solution undergo a condensation reaction to produce pymetrozine acid salt, after the reaction is qualified, the pymetrozine acid salt is subjected to alkali neutralization, and the product is treated to form a pymetrozine raw drug. The method utilizes a method of condensation and then neutralization to replace the existing method of neutralization and then condensation, produces stable aminotriazone acid salt, greatly reduces side reactions caused by free aminotriazone instability and decomposition, reduces impurities, improves pymetrozine product content from 95% to 97% or more, improves a product yield by about 2.0-5.0%, improves a raw material conversion rate, is environmentally friendly and can be industrialized easily.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of pesticides, and in particular relates to a preparation method of pymetrozine. Background technique [0002] Pymetrozine belongs to pyridine or triazinone insecticides. It is a brand-new non-biocide insecticide. It was first developed by Ciba-Geigy in Switzerland in 1988. Pests showed excellent control effect. Studies using electropenetration graph (EPG) technology have shown that no matter in drip, feeding or injection experiments, as long as aphids or planthoppers come into contact with pymetrozine, they will immediately produce a stylet blocking effect, stop feeding immediately, and eventually starve to death , and this process is irreversible. Pyridoxone has no knockdown activity and does not produce direct toxicity to insects. Therefore, pymetrozine has an excellent function of blocking insect transmission. Pymetrozine has a wide insecticidal spectrum, has excellent systemic p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 欧阳建峰黄朝纲陈庆磊李明孙静丽张晖孙衍辉
Owner ANHUI YANGZI CHEM
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