A kind of preparation method of lactoforin

A technology of oxflufenapyr and acifluorfen, which is applied in the field of preparation of oxflufenapyr, can solve the problems of increasing the difficulty and capital expenditure of three-waste treatment, increasing the burden of three-waste treatment, complicated post-processing steps, and the like. The effect of eliminating the use of phase transfer catalysts, being easy to recycle and applying, and simplifying post-processing steps

Active Publication Date: 2016-03-23
SHANGYU NUTRICHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, the solvents selected for this reaction are thionyl chloride and toluene, which are dangerous and pollute the environment. The acid-binding agent is triethylamine, which has a strong pungent stench and is explosive , easy to pollute the environment, increase the difficulty and capital expenditure of the three wastes treatment
Secondly, the moisture is not monitored during the reaction process, which is prone to side reactions and impurities
Finally, after the reaction is completed, the post-treatment steps are more complicated, which will easily lead to product loss, lower yield, and increase the burden of three wastes treatment

Method used

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  • A kind of preparation method of lactoforin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Into a 5000ml four-necked reaction bottle equipped with an azeotropic dehydration device, first put 2500ml of ethyl acetate as a solvent, and then add 1000g (2.76mol) of acifluorfen, 170g (3.02mol) of potassium hydroxide flakes, 2- Ethyl chloropropionate 440g (3.22mol). After the casting is completed, the temperature is raised, and the water generated by the reaction is removed by azeotropic dehydration. Keep warm at 80-85°C, and dehydrate the system while reacting. After the reaction of acifluorfen is complete, evaporate the ethyl acetate at a vacuum degree of -0.095MPa and a liquid temperature of ≦80°C, and finally pass through hot filtration (60 ~80°C), and the by-product potassium chloride was filtered off to obtain lactofen-methyl technical product, with an HPLC purity (retention time consistent with the standard product) of 88.3% and a yield of 98.2%.

[0026] The reaction formula is as follows

[0027]

Embodiment 2

[0029] Put 2500ml of solvent toluene into a 5000ml four-necked reaction bottle equipped with an azeotropic dehydration device, and then add 1000g (2.76mol) of acifluorfen, 170g (3.02mol) of potassium hydroxide, 2-chloropropane Ethyl acetate 440g (3.22mol). After the casting is completed, the temperature is raised, and the water generated by the reaction is removed by azeotropic dehydration. Keep warm at 90-100°C, and dehydrate the system while reacting. After the reaction of acifluorfen is complete, evaporate the toluene at a vacuum degree of -0.095MPa and a liquid temperature of ≦90°C, and finally pass through hot filtration (60-80 °C), and the formed by-product potassium chloride was filtered off to obtain lactofen-methyl technical product, with a HPLC purity (retention time consistent with the standard product) of 86.8% and a yield of 94.5%.

Embodiment 3

[0031] In a 5000ml four-necked reaction flask equipped with an azeotropic dehydration device, first put 2500ml of ethyl acetate as a solvent, and then add 1000g (2.76mol) of acifluorfen, 121g (3.02mol) of sodium hydroxide flakes, 2- Ethyl chloropropionate 440g (3.22mol). After the casting is completed, the temperature is raised, and the water generated by the reaction is removed by azeotropic dehydration. Keep warm at 80-85°C, dehydrate the system while reacting. After the reaction of acifluorfen is complete, evaporate the ethyl acetate at a vacuum degree of -0.095MPa and a liquid temperature of ≦80°C, and finally pass through hot filtration (60 ~80°C), and the formed sodium chloride was filtered off to obtain lactofen-methyl technical product, with a HPLC purity (retention time consistent with the standard product) of 85.3% and a yield of 93.2%.

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Abstract

The invention discloses a preparation method of lactofen. The preparation method of lactofen comprises the following steps: carrying out esterification reaction on acifluorfen and 2-ethyl chloropropionate in an organic solvent in the presence of acid-binding agents, thereby obtaining the lactofen after complete reaction and aftertreatment, wherein the acid-binding agents are at least one of potassium hydroxide, sodium hydroxide, sodium tripolyphosphate, borax anhydrous, CaO, sodium metasilicate, sodium orthosilicate and sodium acetate. According to the invention, special acid-binding agents are selected for replacing potassium carbonate and triethylamine, so that carbon dioxide gas is prevented from generating; the reaction system is more stable; meanwhile, the emission of pollutants is reduced; the environment is protected.

Description

technical field [0001] The invention belongs to the field of synthesizing pesticide technical materials, and in particular relates to a preparation method of lactoforin. Background technique [0002] Lactoforin is a diphenyl ether selective pre-emergence and post-emergence herbicide, which is used to control broad-leaved weeds in cereal crops, corn, cotton, peanut, tomato, rice, and soybean fields. At present, the synthesis methods of lactoferin reported in the literature mainly contain the following three kinds: [0003] Chinese patent CN200710112819.7 discloses a method for preparing high-content lactofen-methyl, in which acifluorfen and ethyl 2-chloropropionate are dissolved in heat, and 2-chloropropionate is added dropwise at 80-85°C. In the mixture of ethyl chloropropionate and potassium carbonate, after the dropwise addition, add the catalyst at 90-95°C, then keep it at 90-95°C for 6-8h, measure the reaction end point by HPLC, filter, add water and wash the filtrate u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/59C07C201/12
Inventor 陈国斌张远冯应江梁俊芳温沛宏陈佳易王晓光王红福王满李伯文陈均坤
Owner SHANGYU NUTRICHEM
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