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Improved synthesis method for glufosinate and analogue thereof

An analogue, glufosinate-ammonium technology, applied in the field of synthesis of glufosinate-ammonium and its analogues, can solve problems such as difficult to meet production requirements, harsh processing and manufacturing process requirements, and high risk, so as to reduce the cost of three wastes treatment and reduce production Cost, the effect of reducing the production of three wastes

Inactive Publication Date: 2012-04-04
JIANGSU YOUTH CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis process is at 500-600°C. If the control is unstable, it is easy to produce yellow phosphorus and phosphine, which are very easy to be natural, which is very dangerous.
In addition, the material is highly corrosive, and there are strict requirements on the material selection and manufacturing process of the reaction equipment. The current domestic processing and manufacturing level is difficult to meet the production requirements.

Method used

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  • Improved synthesis method for glufosinate and analogue thereof
  • Improved synthesis method for glufosinate and analogue thereof
  • Improved synthesis method for glufosinate and analogue thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In a 500ml four-neck flask, add 23.5g of fresh magnesium chips (0.98mol), add THF100g, heat to 35°C and add 1g of methyl bromide dropwise for initiation. Chloromethane 49.5g (0.98mol). The process of passing through the chloromethane maintains a slight reflux state, and maintains a slight reflux state for 2 hours at the end of the passage, until there is almost no visible magnesium chips, and it is ready for use.

[0041] Add 110.7g (0.67mol) of triethyl phosphinate to another 1000ml four-neck flask, add 6g of caprolactam, add 45.8g (0.33mol) of phosphorus trichloride dropwise at 20-25°C, and keep warm for 2 hours after the dropping Diethyl chlorophosphonite is obtained.

[0042] After the above is completed, under strong stirring, add the Grignard reagent dropwise into the diethyl chlorophosphonite, the temperature of the addition is controlled at -10~-5°C, and the drop is completed within 3~4 hours. After the dropwise addition, 2.0 g of dry hydrogen chloride gas was...

Embodiment 2

[0044] Into a 500ml four-neck flask, add 23.2g of fresh magnesium chips (0.965mol), add THF100g, heat to 35°C and add 1g of methyl bromide dropwise for initiation. Chloromethane 48.7g (0.965mol). The process of passing through the chloromethane maintains a slight reflux state, and maintains a slight reflux state for 2 hours at the end of the passage, until there is almost no visible magnesium chips, and it is ready for use.

[0045] Add 110.7g (0.67mol) of triethyl phosphinate to another 1000ml four-neck flask, add 6g of hexamethylphosphonic acid triamide, add dropwise 45.8g (0.33mol) of phosphorus trichloride at 20-25°C, At the end of the dropwise addition, keep warm for 2 hours to obtain diethyl chlorophosphonite.

[0046] After the above is completed, add the Grignard reagent dropwise into the diethyl chlorophosphonite under strong stirring, and the dropping temperature is controlled at -10~-5°C, and the drop is completed in 4~6hr. After the dropwise addition, 5.0 g of dry ...

Embodiment 3

[0049] Add 11.42g of freshly distilled acrolein (0.204mol) dropwise to a mixture of 27.2g of diethyl methylphosphinate (0.2mol) and 46g of ethanol (1mol) under vigorous stirring at 20-30°C, dropwise The adding time is controlled for about 2 hours, and the dropping temperature is controlled at 15-20°C. After the dropwise addition, continue the heat preservation reaction at this temperature for 2 hours, and then recover the ethanol under negative pressure to 90°C / -0.09Mpa. 20g of 5% hydrochloric acid was added dropwise to the residue at 25-30°C, and the reaction was continued at this temperature for 2 hours, and then the ethanol produced by hydrolysis was removed under negative pressure to 60°C / -0.09Mpa. Add the residual material from the precipitation to 9.8g sodium cyanide (0.2mol) and 16.05g ammonium chloride (0.3mol) in 80ml 25% ammonia solution drop by drop, the dropping temperature is controlled at 20-25°C, and the dropping time is controlled for 2hr After the dropwise ad...

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Abstract

The invention discloses a comprehensive method for synthesizing glufosinate and analogue thereof by using phosphorus trichloride, triethyl phosphate and chloromethane as initiative raw materials. The method comprises the following steps of: performing Grignard, disproportionation and coupling; introducing a proper amount of hydrogen halide; and synthesizing to obtain two intermediates, namely methyl diethyl phosphate (intermediate I) and methyl phosphinate (intermediate II), wherein the two intermediates can synthesize the glufosinate and the analogue thereof. By the method, the glufosinate and the analogue thereof are synthesized by completely utilizing the methyl diethyl phosphate and the methyl phosphinate synthesized by a Grignard route; yield is increased; production cost is reduced; and three wastes are reduced.

Description

technical field [0001] The invention relates to a synthesis method of a compound, in particular to a synthesis method of glufosinate-ammonium and its analogues. Background technique [0002] Glufosinate-ammonium (glufosinate-ammonium) was developed and produced by Hearst (now Bayer, Germany), chemical name 4-[hydroxy (methyl) phosphono]-DL-homoalanine, other name glufosinate-ammonium salt , Basta, Buster, etc., are phosphonic acid herbicides, glutamine synthesis inhibitors, non-selective 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, safe for crops, not easy to drift, wide herbicidal spectrum, high activity, less dosage, less environmental pressure, rapid herbicide, can quickly kill more than 100 species of Gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 戚明珠王宝林王东朝孔勇杨凡汪国庆
Owner JIANGSU YOUTH CHEM
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