Supercharge Your Innovation With Domain-Expert AI Agents!

High-purity fipronil preparation method

A fipronil and high-purity technology is applied in the field of preparation of high-purity fipronil, which can solve the problems such as the need to improve the overall yield and the long operation steps, and achieve the effects of conventional equipment, easy operation, and high product yield and purity.

Inactive Publication Date: 2018-04-27
JIANGSU TUOQIU AGRI CHEM CO LTD
View PDF5 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route is the route adopted in industry at present, but the operation steps are longer, and the overall yield needs to be improved

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • High-purity fipronil preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under the micro-vacuum condition with a vacuum degree of -0.1Mpa, 120kg of trifluoromethylthionyl chloride, 450kg of 5-amino-3-cyano-1-(2,6-dichloro-4- Trifluoromethylphenyl) pyrazole, 10kg catalyst trimethylbenzyl ammonium chloride and 1900kg solvent ethylene dichloride, after reacting at 40 ℃ for 1.5 hours, add 120kg trifluoromethylthionyl chloride again, after adding After continuing the insulation reaction for 10 hours, the reaction solution was added to 1000kg of water, allowed to stand for stratification, and centrifuged to filter, and the filtrate was distilled to reclaim ethylene dichloride to recover and apply mechanically to obtain 560kg of filter cake A, then add 560kg of butyl acetate and 2240kg of toluene, and heat up to 85°C, stir until completely dissolved, then lower the temperature to 0°C, keep it warm for 3 hours, then centrifuge, and dry the filter cake B to obtain 450kg of fipronil. The purity of fipronil is determined to be 98%, and the yield is 88....

Embodiment 2

[0028] Under the micro-vacuum condition with a vacuum degree of -0.08Mpa, 110kg of trifluoromethylthionyl chloride, 470kg of 5-amino-3-cyano-1-(2,6-dichloro-4- Trifluoromethylphenyl) pyrazole, 10kg catalyst trimethylbenzyl ammonium chloride and 1500kg solvent ethylene dichloride, after reacting at 35 ℃ for 2 hours, add 110kg trifluoromethylthionyl chloride again, after adding After continuing the insulation reaction for 9 hours, the reaction solution was added to 1000kg of water, allowed to stand for stratification, centrifuged, and the filtrate was distilled to recover dichloroethane and used mechanically to obtain 548kg of filter cake A. 88°C, stir until completely dissolved, then lower the temperature to 2°C, keep it warm for 2 hours, then centrifuge, and dry the filter cake B to obtain 443kg of fipronil. The purity of fipronil is determined to be 97.6%, and the yield is 90.3%.

Embodiment 3

[0030] Under the micro-vacuum condition with a vacuum degree of -0.05Mpa, 125kg of trifluoromethylthionyl chloride, 430kg of 5-amino-3-cyano-1-(2,6-dichloro-4- Trifluoromethylphenyl) pyrazole, 10kg catalyst trimethylbenzyl ammonium chloride and 2000kg solvent ethylene dichloride, after reacting at 45 ℃ for 1 hour, add 125kg trifluoromethylthionyl chloride again, after adding After continuing the heat preservation reaction for 12 hours, add the reaction solution into 1000kg of water, let it stand for stratification, centrifugally filter, and distill the filtrate to recover dichloroethane and apply it mechanically to obtain 578kg of filter cake A, then add 867kg of n-hexane and 2601kg of toluene, and heat up to 90°C , stirred until completely dissolved, lowered the temperature to 5°C, kept the temperature for 5 hours and then centrifuged, and dried the filter cake B to obtain 458kg of fipronil. The purity of fipronil was determined to be 98.2%, and the yield was 89.7%. .

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 provides a high-purity fipronil preparation method. The method includes: under a micro vacuum condition, sequentially adding trifluoromethyl sulfinyl chloride, 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl)pyrazole, catalyst trimethylbenzyl ammonium chloride and solvent dichloroethane into a reaction kettle, adding trifluoromethyl sulfinyl chloride again after reaction for1-2h at 35-45 DEG C, continuing thermal reaction for 9-12h, adding reaction liquid into water, standing for layering, centrifugally filtering, distilling filtrate to recover dichloroethane for recycling and reusing, adding a filter cake A into mixed solvent, heating to 85-90 DEG C, stirring to dissolve completely, cooling for crystallization, centrifugally separating, and drying a filter cake B to obtain fipronil. A fipronil preparation process is simple and easy in operation; by mixed solvent recrystallization for fipronil purification, high fipronil yield and purity and uniformity in product particle size are realized.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and in particular relates to a preparation method of high-purity fipronil. Background technique [0002] Fipronil was developed by the French company Rhône-Planck from 1987 to 1989, and was registered in my country in 1992. After years of development, it has developed into a high-efficiency insecticide that has attracted much attention. Fipronil interferes with the pathway of chloride ions through GABA-mediated chloride channels, disrupting normal central nervous system activity and causing death in individuals at sufficient doses. Because of this unique mechanism of action, fipronil has significant characteristics different from conventional insecticides. A large number of test results have proved that the insecticide is resistant to pests including Hemiptera, Lepidoptera, Thysanoptera, Coleoptera, etc., as well as to cyclopentadiene, pyrethroid, and carbamate insecticides All pest...

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): C07D231/44
CPCC07D231/44
Inventor 廖大章廖大泉孙伯文姚舜华
Owner JIANGSU TUOQIU AGRI CHEM CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com