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Preparation method of glufosinate

A technology of glufosinate-ammonium and compound, which is applied in the field of preparation of glufosinate-ammonium, can solve the problems of cumbersome reaction steps, harsh reaction conditions, and many waste acids, and achieve the effect of simple and quick operation, fewer reaction steps, and high yield

Active Publication Date: 2014-03-26
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are many technical routes related to glufosinate-ammonium at home and abroad. Although glufosinate-ammonium can be obtained, the reaction conditions are relatively harsh, the reaction steps are loaded down with trivial details, the reaction time is too long, the purification of reactants is difficult and the by-product inorganic salts are too much, waste Too much acid, these undoubtedly bring certain limitations to large-scale production
For example, the preparation method invented by Li Xukun (CN103288874A) and others has the following disadvantages: for example, the high-cost raw material hydantoin requires a high temperature of 100°C for the reaction, and the hydrolysis of hydantoin derivatives in inorganic acids requires at least reflux Thirty hours, and the yield and content of the finished glufosinate-ammonium product are not high, and the value of large-scale production is not great

Method used

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  • Preparation method of glufosinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step (1): Preparation of the compound shown in formula (II)

[0026] Add 4.9 g of crushed sodium cyanide and 50 ml of dried chloroform into a 500 ml dry three-necked flask, stir and heat to 50°C, and slowly add 13.4 g of the compound represented by formula (I) and 67 ml of dried The mixed solution of chloroform, the dropping temperature is controlled at 50°C-60°C, after the dropwise addition, the heat preservation reaction is carried out for 2 hours, after the reaction is completed, the solvent chloroform is distilled off under reduced pressure, cooled and filtered, and dried to obtain 18.3 grams of white solid powder , which is the compound represented by formula (II).

[0027] Step (2): Preparation of the compound shown in formula (Ⅲ)

[0028] In a 250 ml three-necked flask, add 122 grams of 30% hydrochloric acid, stir, and then add 18.3 grams of the compound shown in formula (II). Add hydrogen chloride, stir and react at this temperature for about 1.5 hours, then h...

Embodiment 2

[0032] Step (1): Preparation of the compound shown in formula (II)

[0033] Add 6.8 g of crushed potassium cyanide and 50 ml of dried chloroform into a 500 ml dry three-necked flask, stir and heat to 60°C, and slowly add 18.5 g of the compound represented by formula (I) and 67 ml of dried For the mixed solution of chloroform, the dropwise addition temperature is controlled at 55°C-65°C. After the dropwise addition, the heat preservation reaction is carried out for 2 hours. After the reaction is completed, the solvent chloroform is distilled off under reduced pressure, cooled, filtered, and dried to obtain 25.3 grams of white solid powder, namely It is a compound represented by formula (II).

[0034] Step (2): Preparation of the compound shown in formula (Ⅲ)

[0035] In 250 milliliters of three ports, add 122 grams of 30% hydrochloric acid, stir, then add 25.3 grams of the compound shown in formula (II), after the addition is complete, the reaction system is rapidly reduced to...

Embodiment 3

[0039] Step (1): Preparation of the compound shown in formula (II)

[0040]Add 4.9 g of crushed sodium cyanide and 50 ml of dried dichloroethane into a 500 ml dry three-necked flask, stir and heat to 50°C, and slowly add 13.4 g of the compound represented by formula (I) and 67 Milliliters of dried dichloroethane mixed solution, the dropwise addition temperature is controlled at 50°C-60°C, after the dropwise addition, keep warm for 2 hours, after the reaction, the solvent dichloroethane is distilled off under reduced pressure, cooled and filtered, After drying, 17.5 g of white solid powder was obtained, which was the compound represented by formula (II).

[0041] Step (2): Preparation of the compound shown in formula (Ⅲ)

[0042] In a 250 ml three-neck flask, add 150 g of 30% phosphoric acid, stir, then add 17.5 g of the compound shown by formula (II), heat to 110°C, and react for 10 hours. Then the water was evaporated under reduced pressure, and evaporated to dryness as muc...

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Abstract

The invention relates to a preparation method of glufosinate. The preparation method comprises the following steps: with a compound represented by a formula (I) as a starting material, reacting the compound represented by the formula (I) with cyanide RCN to obtain ketone nitrile; then hydrolyzing ketone nitrile in the presence of an acidic substance and water so as to obtain ketoacid; and reacting ketoacid successively with ammonia gas and hydrogen under the action of a catalyst so as to obtain glufosinate; wherein the compound represented by the formula (I) is cyclic phosphonic acid anhydride. The preparation method in the invention has the advantages of simple process, convenient operation, high product purity, high yield, no need for repeated recrystallization, ect.; and the final product of the preparation method is directly glufosinate ammonium, the step of converting glufosinate chloride into glufosinate ammonium is omitted, so the method has great economic benefit and is suitable for industrialization production.

Description

technical field [0001] The invention relates to a preparation method of glufosinate-ammonium. Background technique [0002] Glufosinate ammonium, alias: glufosinate; 4-[hydroxy(methyl)phosphono]-DL-homoalanine; glufosinate ammonium salt; 2-amino-4-[hydroxy(methyl) )phosphono]ammonium butyrate; 4-(hydroxy(methyl)phosphono)-DL-homoalanine; bialaphos; glufosinate. CAS number: 77182-82-2, molecular formula: C 5 h 18 N 3 o 4 P, molecular weight: 215.19. Its structural formula is: [0003] [0004] Glufosinate-ammonium is a highly efficient, low-toxic, non-selective contact-type organic phosphine herbicide with partial systemic effect, which was first developed by the German Hoechst company. [0005] At present, there are many technical routes related to glufosinate-ammonium at home and abroad. Although glufosinate-ammonium can be obtained, the reaction conditions are relatively harsh, the reaction steps are loaded down with trivial details, the reaction time is too long...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 闫立单余强韩士芳顾松山陶亚春吕宜飞龚建华
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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