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Synthesis method for glufosinate and analogue thereof

An analogue, glufosinate-ammonium technology, applied in the field of compound synthesis, can solve problems such as high risk, difficult to meet production requirements, and harsh manufacturing process requirements, so as to reduce the generation of three wastes, reduce the cost of three wastes treatment, and improve The effect of synthesis yield

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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  • Synthesis method for glufosinate and analogue thereof
  • Synthesis method for glufosinate and analogue thereof
  • Synthesis method for glufosinate and analogue thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 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.

[0037] 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.

[0038] 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, continue to keep warm for 3 hours. Af...

Embodiment 2

[0040] 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.

[0041] 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.

[0042] 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, continue to...

Embodiment 3

[0049] Add 11.42g of freshly distilled acrolein (0.204mol) to 20.81g of acetic anhydride (0.204mol) at 20-30°C, and mix well. Then it was added dropwise to a mixture of 27.2g diethyl methylphosphonite (0.2mol) and 9.2g ethanol (0.2mol) under vigorous stirring, the dropping time was controlled for about 2hr, and the dropping temperature was controlled at 15-20°C. After the dropwise addition, continue the heat preservation reaction at this temperature for 2 hours, and then remove the light components under negative pressure to 100°C / -0.095Mpa. Add the residual material dropwise to 9.8g of sodium cyanide (0.2mol) and 21.4g of ammonium chloride (0.4mol) in 100ml of 25% ammonia solution. After the addition was completed, the insulation reaction was continued for 4 hr. The material was added to 400ml of 30% hydrochloric acid without separation, heated to reflux for 3 hours, and dehydrated to 60°C / -0.095Mpa under negative pressure. Add 120g of methanol and 15g of deionized water to...

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Abstract

The invention provides a synthesis method for glufosinate shown as a formula (V) and an analogue thereof. The method comprises the following steps of: preparing an intermediate such as methyl diethyl phosphate by Grignard, disproportionation and coupling and with phosphorus trichloride, triethyl phosphate and chloromethane as initiative raw materials; condensing the methyl diethyl phosphate, anhydride and acrolein substances; performing Strecker reaction and hydrolysis and thus obtaining the glufosinate and the analogue thereof. In the synthesis method, the reaction condition is mild; safety is high; and yield is obviously increased.

Description

technical field [0001] The invention relates to a synthesis method of a compound, in particular to a synthesis method of the herbicide glufosinate-ammonium and its analogues. Background technique [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, safe for crops, not easy to drift, wide herbicidal spectrum, high activity, less dosage, less environmental pressure, ...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 戚明珠王宝林王东朝孔勇黄东进蒋贤梅
Owner JIANGSU YOUTH CHEM
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