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Environment-friendly novel technology for synthesizing high content nicosulfuron

A nicosulfuron-methyl, high-content technology, applied in the field of pesticides, can solve the problems of high labor intensity, waste of energy, and potential safety hazards, and achieve the effects of shortening reaction time, reducing labor intensity, and reducing energy waste

Inactive Publication Date: 2014-01-01
ANHUI FENGLE AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process requires two steps of reaction, and the intermediate needs to be dried before it can enter the final step of condensation reaction. At the same time, the last step of condensation reaction needs to use a rectification tower, and the condensation reaction time needs more than ten hours. Therefore, the process and equipment are complex and the reaction time is Long, many operation steps, high labor intensity, waste of energy, and the generated by-product alcohols destroy the generated nicosulfuron, the content and yield are not high, and the safety hazard is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Put quantitative N,N-dimethyl-2-aminosulfonyl-pyridinamide, 2-amino-4,6-dimethoxypyrimidine into a 500ml four-necked flask equipped with a thermometer, a stirrer and a condenser , Catalyst 1 and dichloromethane, after stirring at room temperature for 30 minutes, start to drop weighed phenyl chloroformate, add catalyst 2 after dripping, heat up to reflux, keep warm for 3 hours, and after the reaction finishes, The nicosulfuron product was obtained, with a yield of 90.7% based on N,N-dimethyl-2-aminosulfonyl-pyridinamide, and a product content of 98.7%.

Embodiment 2

[0011] Put quantitative N,N-dimethyl-2-aminosulfonyl-pyridinamide, 2-amino-4,6-dimethoxypyrimidine into a 500ml four-necked flask equipped with a thermometer, a stirrer and a condenser , Catalyst 1 and ethylene dichloride, after stirring at room temperature for 30 minutes, start to drop quantitatively the diphenyl carbonate solution dissolved in ethylene dichloride, add catalyst 2 after dropping, heat up to reflux, and keep the temperature for 3.5 hours, After the completion of the reaction, the product of nicosulfuron was obtained after post-treatment. The yield calculated by N,N-dimethyl-2-aminosulfonyl-pyridinamide was 90.5%, and the product content was 98.2%.

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PUM

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Abstract

The invention provides an environment-friendly novel technology for synthesizing high content nicosulfuron. According to the invention, phenyl chloroformate or diphenyl carbonate is adopted to substitute ethyl chloroformate or methyl clhlorofonmate, which is a toxic substance; organic catalyst or inorganic catalyst is adopted; dichloromethane, dichloroethane, or acetonitrile is used as a solvent; N,N-dimethyl-2-amidosulfonyl-picolinamide, 2-amidogen-4,6,-dimethoxy-pyrimidine, catalyst I, and the solvent are added into a reaction kettle as whole; adding phenyl chloroformate or diphenyl carbonate and catalyst II sequentially at room temperature; performing heating reflux to obtain the product. The yield is above 90%, and the content is above 98%.

Description

technical field [0001] The invention belongs to the technical field of pesticides, and in particular relates to a new synthesis process of high-content nicosulfuron. Background technique [0002] The current domestic method for synthesizing nicosulfuron is mainly to react N,N-dimethyl-2-aminosulfonyl-pyridinamide with the highly toxic substance ethyl chloroformate (or methyl ester) to generate an intermediate, and the intermediate is then Condensation reaction with 2-amino-4,6-dimethoxypyrimidine to generate the original drug of nicosulfuron. The process requires two steps of reaction, and the intermediate needs to be dried before it can enter the final step of condensation reaction. At the same time, the last step of condensation reaction needs to use a rectification tower, and the condensation reaction time needs more than ten hours. Therefore, the process and equipment are complex and the reaction time is Long, many operation steps, high labor intensity, waste of energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 周康伦吴永虎苏朝辉凌朵朵陈克付
Owner ANHUI FENGLE AGROCHEM
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