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

Fenoxaprop-p-ethyl and preparation method thereof

A technology of oxaflufen-ethyl and phenoxybenzoxazole, which is applied in the field of low-toxicity herbicide oxaflufen-ethyl and its preparation, can solve problems such as reducing product yield and quality, and achieve higher content Effect

Inactive Publication Date: 2013-05-22
JIANGSU XUE BAO DAILY CHEM CO
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis reaction of fenoxaprop-p-ethyl is a solid-liquid phase reaction, and the traditional synthesis method and equipment have serious deficiencies in this reaction, which greatly reduces the product yield and quality

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

[0010] Put 160ml of solvent, 30g of 6-chloro-2-(p-hydroxy)phenoxybenzoxazole, and 30g of acid-binding agent into the condensation kettle in turn, heat up and dehydrate until the water separator is dry, then add 0.5g of catalyst , at 100 o c Add 32g of ethyl p-toluenesulfonyl propionate, the dropwise addition time is 2 hours, keep warm for 6 hours after adding, after the central control is qualified, cool for 60-90 o c Add water, send the water layer to the three-waste station, filter the material to the water washing kettle, wash with water until neutral, desolvate under reduced pressure, vacuum degree ≤ -0.095 MPa, remove until there is no fraction, after the desolventization is completed, turn off the vacuum and vent , cooled to 70~90 o c Add 80ml of ethanol to dissolve the material, cool and crystallize, and the temperature drops to -2~2 o About c, the material is discharged and centrifuged, and the product is dried to obtain 37.4g of finished product, with a content of...

example 2

[0011] Example 2: Throw 160ml of solvent, 30g of 6-chloro-2-(p-hydroxy)phenoxybenzoxazole, and 35g of acid-binding agent into the condensation kettle in sequence, heat up and dehydrate, and then add Catalyst 1.5g, at 90 o c Add 34 g of ethyl p-toluenesulfonyl propionate dropwise, the time for the dropwise addition is 2.5 hours, keep warm for 8 hours after the addition, and cool for 60-90 minutes after the central control is qualified. o c Add water, send the water layer to the three-waste station, filter the material to the water washing kettle, wash with water until neutral, desolvate under reduced pressure, vacuum degree ≤ -0.095 MPa, remove until there is no fraction, after the desolventization is completed, turn off the vacuum and vent , cooled to 70~90 o c Add 80mL ethanol to dissolve the material, cool and crystallize, and the temperature drops to -2~2 o About c, the discharge is centrifugal, and the product is dried to obtain finished product 37.1g, content 97.0%, e...

example 3

[0012] Example 3: Throw 160ml of solvent, 30g of 6-chloro-2-(p-hydroxy)phenoxybenzoxazole, and 35g of acid-binding agent into the condensation kettle in turn, heat up and dehydrate, and then add Catalyst 1.5g, at 90 o c Add 34g of ethyl p-toluenesulfonyl propionate, dropwise adding time is 2.5 hours, keep warm for 8 hours, after the central control is qualified, cool for 60-90 o c Add water, send the water layer to the three-waste station, filter the material to the water washing kettle, wash with water until neutral, desolvate under reduced pressure, vacuum degree ≤ -0.095 MPa, remove until there is no fraction, after the desolventization is completed, turn off the vacuum and vent , cooled to 70~90 o c Add 80mL ethanol to dissolve the material, cool and crystallize, and the temperature drops to -2~2 o About c, the discharge is centrifugal, and the product is dried to obtain finished product 37.7g, content 97.3%, effective body content 99.5%, yield 87.5%.

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 relates to fenoxaprop-p-ethyl and a preparation method thereof. The fenoxaprop-p-ethyl is mainly prepared from 6-chloro-2-(p-hydroxy)phenoxy benzoxazole, ethyl p-methylbenzenesulfonyl propionate, solvent, an acid binding agent and a catalyst. The method comprises the following steps: sequentially adding the solvent, the 6-chloro-2-(p-hydroxy)phenoxy benzoxazole and the acid binding agent into a condensation kettle, and heating to dewater until no water exists; adding the catalyst, dropwisely adding the ethyl p-methylbenzenesulfonyl propionate at 80-120 DEG C, and keeping the temperature for 2-12 hours after the dropwise addition is finished; after intermediate control is qualified, cooling to 60-90 DEG C, washing with water to neutral, and performing reduced pressure desolvation at a vacuum degree no more than -0.095 MPa until no fraction exists; and after the desolvation is finished, switching off the vacuum, emptying, cooling to 70-90 DEG C, adding ethanol to enable the material to be subjected to solvent-out crystallization, cooling to (-2)-2 DEG C, discharging, centrifuging, and drying the product. The invention can effectively improve the product yield and quality, is simple to operate and causes less pollution to the environment.

Description

technical field [0001] The invention relates to a low-toxicity herbicide fenoxaprop-p-ethyl and a preparation method thereof, which is mainly used for controlling dicotyledon crops such as soybean, peanut, rapeseed, cotton, sugar beet, flax, potato, vegetable field and mulberry orchard. leaf weeds. Background technique [0002] Fenoxaprop-p-ethyl is a new heterocyclic herbicide of phenoxycarboxylic acid type, which has the characteristics of high efficiency, low toxicity, and little environmental pollution; Such as Kan Mai Niang, wild oats, foxtail and other weeds, have a good control effect. Its preparation method and key preparation equipment play a key role in the content of its active ingredients. The synthesis reaction of fenoxaprop-p-ethyl is a solid-liquid phase reaction, and the traditional synthesis method and equipment have serious deficiencies in this reaction, which greatly reduces the product yield and quality. Contents of the invention [0003] The purpose...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/58
Inventor 童星杜永卫
Owner JIANGSU XUE BAO DAILY CHEM CO
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

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com