Preparation method of environment-friendly fomesafen

A kind of fomesafen, environment-friendly technology, applied in the field of synthesis and preparation of fomesafen, can solve problems such as pollution, achieve the effects of improving conversion speed, easy transportation and storage, and mild reaction conditions

Pending Publication Date: 2022-01-18
山东科源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of environmentally friendly fomesafen, by changing the acylating agent and the synthesis process, the problem of environmental pollution caused by traditional phosphorus oxychloride as an acylating agent is solved, and a safe and environmentally friendly fluorine Synthesis and preparation of sulfafen, and at the same time, through the design of the catalyst, the conversion rate and reaction speed are improved while reducing the influence of the color of the metal chloride salt itself on product quality

Method used

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  • Preparation method of environment-friendly fomesafen
  • Preparation method of environment-friendly fomesafen
  • Preparation method of environment-friendly fomesafen

Examples

Experimental program
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Effect test

Embodiment 1

[0041] refer to figure 1 , using nitrate 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid, methylsulfonamide and solid phosgene to synthesize fluorosulfonamide under the action of dichloroethane grass ether. 5-[2-Chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid dichloroethane was extracted and then transferred to the reaction kettle, 5-[2-chloro-4-(trifluoromethyl) The input amount of methyl)phenoxyl]-2-nitrobenzoic acid is 383 parts, and after dichloroethane is qualified with water, the input amount of methylsulfonamide is 114 parts, and solid light is added at a uniform speed, and the input of solid phosgene The amount is 118 parts, the temperature is kept below 90°C, after the addition of solid light, keep it warm for 2 hours, add the seed crystal and continue the reaction at 100-120°C, the reaction time is 12h, then lower the temperature, add water, filter, and dry to get fluorosulfonamide Finished product of grass ether. The mass fraction of the finish...

Embodiment 2

[0044] refer to figure 1 , using nitrate 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid, methylsulfonamide and solid phosgene to synthesize fluorosulfonamide under the action of dichloroethane grass ether. 5-[2-Chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid dichloroethane was extracted and then transferred to the reaction kettle, 5-[2-chloro-4-(trifluoromethyl) The input amount of methyl)phenoxyl]-2-nitrobenzoic acid is 383 parts, and after dichloroethane is qualified with water, the input amount of methylsulfonamide is 104 parts, and solid light is added at a uniform speed, and the input of solid phosgene The amount is 109 parts, the temperature is kept below 90°C, after the addition of solid light, keep it warm for 2 hours, add seed crystals and continue the reaction at 100-120°C, the reaction time is 12h, then lower the temperature, add water, filter, and dry to obtain fluorosulfonamide Finished product of grass ether. The mass fraction of the finish...

Embodiment 3

[0047] refer to figure 1, using nitrate 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid, methylsulfonamide and solid phosgene to synthesize fluorosulfonamide under the action of dichloroethane grass ether. 5-[2-Chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid dichloroethane was extracted and then transferred to the reaction kettle, 5-[2-chloro-4-(trifluoromethyl) The input amount of methyl)phenoxyl]-2-nitrobenzoic acid is 383 parts, and after dichloroethane is qualified with water, the input amount of methylsulfonamide is 114 parts, and solid light is added at a uniform speed, and the input of solid phosgene The amount is 118 parts, the temperature is kept below 90 ° C, after the addition of solid light, keep it warm for 2 hours, add 8 parts of catalyst to the reaction at 100-120 ° C, remove the catalyst after 8 hours of reaction, continue to react for a total time of 10 hours, then lower the temperature and add water , filtered, and dried to obtain the fin...

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Abstract

The invention discloses a preparation method of environment-friendly fomesafen, and relates to the field of synthesis of fomesafen. The fomesafen is synthesized from 5-[2-chloro-4-(trifluoromethyl) phenoxy]-2-nitrobenzoic acid, methanesulfonamide and triphosgene under the action of dichloroethane. According to the invention, by changing an acylating agent and a synthesis process, the problem of environmental pollution caused by taking phosphorus oxychloride as the acylating agent in the prior art is solved, and safe and environment-friendly synthesis and preparation of fomesafen are realized; and by improving the catalyst, the conversion rate and the reaction speed are improved, and the influence of the color of the chlorinated metal salt on the product quality is reduced.

Description

technical field [0001] The invention relates to the field of fomesafen synthesis, in particular to an environment-friendly synthesis and preparation method of fomesafen. Background technique [0002] Fomesafen, that is, 5-(2-chloro-α,α,α-trifluoro-p-tolyloxy)-N-methylsulfonyl-2-nitrobenzamide; the active ingredient content of the drug is 95%, Appearance Off-white powdery solid. Melting point 218-221°C, density: 1.28g / cm3, vapor pressure <0.1mpa (50°C), it is a highly selective post-emergence herbicide for soybean and peanut fields, which can effectively control broad-leaved soybean and peanut fields Weeds and Cyperus can also be used in orchards and rubber plantations to control broadleaf weeds. It also has a certain control effect on grass weeds. It can be absorbed by the roots and leaves of weeds, causing them to quickly wither and die. Rain 4-6 hours after spraying will not affect the efficacy of the medicine, and it is safe for soybeans. Therefore, the application...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/40C07C311/51B01J29/80
CPCC07C303/40B01J29/80B01J29/763B01J29/76C07C311/51
Inventor 张华叶春霞张明伟原龙腾提云恒
Owner 山东科源化工有限公司
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