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

Synthetic method of diethyl methyl-phosphonite and glufosinate-ammonium

A technology of diethyl methyl phosphonite and diethyl methyl phosphonate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the intermediate methyl Phosphonyl dichloride is extremely unstable, etc., and achieves the effects of high atomic utilization, simple reaction process, and wide application value.

Active Publication Date: 2013-09-25
SHANDONG WEIFANG RAINBOW CHEM
View PDF6 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of these two methods is that the intermediate methyl phosphonyl dichloride is extremely unstable and flammable when exposed to air.

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
  • Synthetic method of diethyl methyl-phosphonite and glufosinate-ammonium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In a 1L autoclave, add 138g of diethyl phosphite and 101g of anhydrous triethylamine, close the autoclave, and use N 2 The air in the kettle was replaced, the temperature was raised to 110°C with stirring, and methyl chloride gas was slowly introduced to maintain the pressure in the kettle at 0.4-0.8 MPa during the reaction. After 4 hours of reaction, the temperature was lowered and the pressure was released, triethylamine hydrochloride was removed by suction filtration, the filtrate was transferred to a 1000 mL four-necked flask, the temperature was cooled to 0 °C with an ice-salt bath, and 200 mL of a THF solution dissolved in 19 g of lithium tetrahydrogen was slowly added dropwise. After the dropwise addition, continue to insulate and stir for 120 min. The temperature was slowly raised for distillation, and 126.1 g of fractions with a boiling point of 120-122°C were collected. The content of diethyl methylphosphonite was detected to be 98.5%, and the yield was 91.3%....

Embodiment 2

[0037] In a 1L autoclave, add 138g of diethyl phosphite and 222g of tri-n-butylamine, close the autoclave, and use N 2 Replace the air in the kettle, stir and raise the temperature to 100°C, and slowly feed in methyl chloride gas to maintain the pressure in the kettle at 0.4-0.8MPa. After reacting for 3 hours, the temperature was lowered and the pressure was released, tributylamine hydrochloride was removed by suction filtration, the filtrate was transferred to a 1000 mL four-neck flask, the temperature was cooled to 5 °C with an ice-salt bath, and 200 mL of a methyl tetrahydrofuran solution dissolved in 19 g of lithium tetrahydrogen was slowly added dropwise. After the dropwise addition, continue to insulate and stir for 90 min. The temperature was slowly raised for distillation, and 120.8 g of fractions with a boiling point of 120-122°C were collected. The content of diethyl methylphosphonite was detected to be 98.8%, and the yield was 87.8%.

Embodiment 3

[0039] In a 1L autoclave, add 138g of diethyl phosphite and 367.5g of triphenylamine, close the autoclave, and use N 2 Replace the air in the kettle, stir and raise the temperature to 120°C, slowly feed in methyl chloride gas to maintain the pressure in the kettle at 0.4-0.8MPa. After reacting for 2 hours, the temperature was lowered and the pressure was released, triphenylamine hydrochloride was removed by suction filtration, the filtrate was transferred to a 1000 mL four-neck flask, the temperature was lowered to 10°C with a cold water bath, and 200 mL of ether solution dissolved in 24 g of sodium hydride was slowly added dropwise. After the dropwise addition, continue to insulate and stir for 60 min. The temperature was slowly raised to distill, and 119.5 g of fractions with a boiling point of 120-122°C were collected. The content of diethyl methylphosphonite was detected to be 98.9%, and the yield was 86.9%.

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 discloses a synthetic method of diethyl methyl-phosphonite and glufosinate-ammonium. The synthetic method comprises the following steps: carrying out a reaction between diethyl phosphite and chloromethane gas in the presence of an acid binding agent to prepare diethyl methylphosphonite, and filtering after reaction, wherein the generated diethyl methylphosphonite exists in a filtrate; dropwisely adding an organic solvent, in which a reducing agent is dissolved, into the filtrate so as to reduce diethyl methylphosphonite into diethyl methyl-phosphonite, distilling a reaction solution after the reaction so as to obtain diethyl methyl-phosphonite, and preparing glufosinate-ammonium by using diethyl methyl-phosphonite as an intermediate. According to the invention, diethyl phosphite is used as a raw material; reaction raw materials are cheap and easily available; the reaction process is simple and easy to operate and is green and environmentally friendly; atom utilization rate is high; quality of the obtained product is good; yield is high; a new idea is provided for the synthesis of glufosinate-ammonium; preparation cost of glufosinate-ammonium is also reduced; and the synthetic method has wide application value.

Description

technical field [0001] The invention relates to a synthesis method of diethyl methylphosphonite and glufosinate-ammonium, in particular to a green and environment-friendly synthesis method of diethyl methylphosphonite and glufosinate-ammonium, and belongs to the technical field of herbicides. technical background [0002] Glufosinate-ammonium (glufosinate-ammonium) was developed and produced by Hearst (now owned by Bayer after several mergers), chemical name 4-[hydroxy (methyl) phosphono]-DL-homoalanine, other name glufosinate-ammonium Ammonium phosphonate, Basta, Buster, etc., are phosphonic acid herbicides, glutamine synthesis inhibitors, non-selective (killing) contact herbicides. It was developed in the 1980s and registered as a herbicide in 1984. Glufosinate-ammonium is a large-tonnage pesticide variety in the world, and it is also the second largest genetically modified crop resistant to herbicides in the world. Low toxicity, relatively safe, easy to degrade in soil,...

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): C07F9/40C07F9/30
Inventor 孙国庆侯永生张杰李志清张利国高国利马华青牟红海杜鹏单春花张艳袁国秀任师涌石爱防褚宝琦李本玉杨辉葛龙飞
Owner SHANDONG WEIFANG RAINBOW CHEM
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