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Concise glufosinate ammonium synthesizing method

A synthesis method and glufosinate-ammonium technology are applied in the chemical industry to achieve the effects of simplified operation steps, good application prospects and reduced labor intensity

Active Publication Date: 2018-11-02
LIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a simple synthetic method for glufosinate-ammonium in view of the problem that highly toxic sodium cyanide needs to be used when synthesizing glufosinate-ammonium in the existing method
Different from the existing method of using diethyl methyl phosphite to prepare glufosinate-ammonium, the present invention can effectively avoid the use of highly toxic chemicals and solve the problem of sodium cyanide application

Method used

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  • Concise glufosinate ammonium synthesizing method
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  • Concise glufosinate ammonium synthesizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 90.67kg (686.5mol) of N-acetyl-2-aminobutenoic acid (97% in absolute content) was dissolved in 200 liters of methyl tetrahydrofuran to obtain the first solution; then the first solution was added dropwise to the methyl In 81.9kg of phosphine dichloride (98%, obtained by rectification), the temperature is controlled within 70-90°C. After the dropwise addition is completed, the reaction solution is kept at 85-90°C for 1 hour, and the sample is tested to prove that the reaction has been completed. , to obtain the second reaction solution; while hot, the second reaction solution is put into another 1000 liter reaction kettle, the temperature is controlled in the range of 0 to 30°C, and under stirring conditions, slowly add 38.2 kilograms of water dropwise, after the dropwise addition is completed, then Add 60 kg of water, then heat up to reflux for 3 to 4 hours to detect that the amide has been hydrolyzed, then slowly add 365 kg of 30% sodium hydroxide to obtain the third re...

Embodiment 2

[0045] Dissolve 90.67kg (686.5mol) of (2S)-N-acetyl-2-aminobutenoic acid (97% in absolute content) in 200 liters of methyl tetrahydrofuran to obtain the first solution; then drop the first solution Add it to 81.9kg of methylphosphine dichloride (98%, obtained by rectification), and control the temperature within 70-90°C. After the dropwise addition, keep the reaction solution at 85-90°C for 1 hour, and take a sample for detection. It is proved that the reaction has been completed, and the second reaction solution is obtained; the second reaction solution obtained is put into another 1000-liter reaction kettle while it is hot, and the temperature is controlled within the range of 0-30°C. Under the condition of stirring, slowly add 38.2 kg of water, dropwise After completion, add 60 kilograms of water again, then heat up to reflux reaction for 3 to 4 hours, detect that the amide has been hydrolyzed, slowly add 365 kilograms of 30% sodium hydroxide to obtain the third reaction sol...

Embodiment 3

[0047] 90.67kg (686.5mol) of N-acetyl-2-aminobutenoic acid (97% in absolute content) was dissolved in 200 liters of methyl tetrahydrofuran to obtain the first solution; then the first solution was added dropwise to the methyl In phosphine dichloride 90kg (98%, rectification gained), temperature is controlled within 65~80 ℃, after dropwise addition is completed, the reaction solution is incubated and reacted for 1 hour at 75~80 ℃, and sampling inspection proves that the reaction has been completed. Obtain the second reaction liquid; put the obtained second reaction liquid into another 1000-liter reaction kettle while it is hot, control the temperature in the range of 0-10°C, and slowly add 38.2 kg of water dropwise under stirring conditions. After the dropwise addition, add 60 kg of water, then heated up to reflux reaction for about 3 hours, detected that the amide had been hydrolyzed, cooled to normal temperature (20-30°C), controlled the temperature at 20°C-30°C, slowly added ...

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Abstract

The invention discloses a concise glufosinate ammonium synthesizing method and aims at solving the problem that an existing method needs to use toxic sodium cyanide to synthesize glufosinate ammonium.Being different from an existing method of using diethyl methyl phosphite to prepare the glufosinate ammonium, the concise glufosinate ammonium synthesizing method disclosed by the invention can effectively avoid using toxic chemicals; thus, the problem of using the sodium cyanide is solved. By means of the synthesizing method, use of toxic chemicals is reduced, operation steps are simplified, equipment investment is reduced, the amount of three wastes is reduced, a requirement for clean production is met, and more environmental friendliness is achieved. Meanwhile, the synthesizing method disclosed by the invention not only can synthesize racemate glufosinate ammonium, but also can synthesize optical pure-chirality glufosinate ammonium, so that the synthesizing method has obvious progressive significance. According to the synthesizing method disclosed by the invention, technique connection is orderly, no solid material is used, convenience in operation is achieved, a technological process is simple, automatic production is achieved, labor intensity of workers is greatly reduced, and a production efficiency is improved; thus, the synthesizing method has a better application prospect and is worth of popularizing and applying in a large scale.

Description

technical field [0001] The invention relates to the field of chemical industry, especially the field of synthesis, and specifically relates to a simple synthesis method of glufosinate-ammonium. The invention provides a method for synthesizing the herbicide glufosinate-ammonium, which can not only be used for the synthesis of racemate glufosinate-ammonium, but also be used for the synthesis of optically pure L-glufosinate-ammonium, which has important significance. Background technique [0002] Glufosinate-ammonium (glufosinate-ammonium) was developed and produced by Hoechest in the 1980s. Its chemical name is 4-[hydroxy (methyl)phosphono]-DL-homoalanine, also known as glufosinate-ammonium ammonium salt , is a phosphoric acid herbicide. In recent years, with the rapid development of domestic glufosinate-ammonium, a variety of synthetic routes have emerged. [0003] Hoechst proposed in the US6359162B1 patent that diethyl methylphosphite and acrolein were reacted to obtain an...

Claims

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Application Information

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IPC IPC(8): C07F9/30C07F9/34
CPCC07B2200/07C07F9/301C07F9/34
Inventor 周波曾柏清邱亮彭启才范谦
Owner LIER CHEM CO LTD
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