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Preparation method of buprofezin

A technology of buprofezin and organic amines, which is applied in the field of preparation of buprofezin, can solve the problems of high ammonia nitrogen content, serious environmental pollution, high solubility and unfavorable hydrogen chloride overflow yield, etc., and achieve the effect of low ammonia nitrogen content and low solubility

Active Publication Date: 2014-06-25
JIANGSU CHANGLONG AGROCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet select one of above-mentioned solvent product HCL to be unfavorable for the overflow of hydrogen chloride and be unfavorable for the raising of productive rate in the solvent that the solubility of one of HCL is higher, select ammonia bicarbonate condensation buprofezin for use, the ammonia nitrogen content in the reaction waste water is higher, and environmental pollution is serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0012] (1) Photochemical reaction: Put 1000ml of solvent dioxane into the photochemical kettle, start stirring, increase the temperature, control the temperature at about 15℃, and add phosgene 300g (96.8%) while adding 240g N-methylaniline dropwise , And then slowly increase the temperature to 50 degrees, maintain a small amount of phosgene during the period, and then use nitrogen to drive off the excess phosgene and hydrogen chloride to obtain N-methylphenylcarbamoyl chloride dioxane solution;

[0013] (2) Chlorination reaction: Add 5g of the catalyst azobisisobutyronitrile to the aforementioned N-methylphenylcarbamoyl chloride dioxane solution, control the temperature of the photochemical kettle at 55°C, and pass 190g of chlorine gas into it to detect N- If the dichloromethylphenylcarbamoyl chloride is greater than 0.5%, the excess chlorine gas and by-product hydrogen chloride are purged with nitrogen to obtain the N-chloromethylphenylcarbamoyl chloride dioxane solution;

[0014]...

Embodiment 2）

[0017] (1) Photochemical reaction: Put 1000ml of chloroform into the photochemical kettle, start stirring, increase the temperature, and control the temperature at about 15℃. While passing in phosgene 300g (96.8%), add 240g of N-methylaniline dropwise, then slowly Slowly increase the temperature to 50°C while maintaining a small amount of phosgene, then use nitrogen to drive off the excess phosgene and hydrogen chloride. After the reaction, the materials are distilled under reduced pressure and the solvent chloroform is removed to obtain N-methylphenylcarbamoyl chloride. ;

[0018] (2) Chlorination reaction: dissolve the aforementioned N-methylphenylcarbamoyl chloride in 300g of N-chloromethylphenylcarbamoyl chloride, add 5g of the catalyst azobisisobutyronitrile, and control the photochemical kettle temperature at 55 190g of chlorine gas is introduced at ℃, and N-dichloromethylphenylcarbamoyl chloride is detected to be greater than 0.5%, and the excess chlorine and by-product hy...

Embodiment 3）

[0022] (1) Photochemical reaction: Put 1000ml of solvent dioxane into the photochemical kettle, start stirring, increase the temperature, control the temperature at about 15℃, and add phosgene 300g (96.8%) while adding 240g N-methylaniline dropwise , And then slowly increase the temperature to 50 degrees, maintain a small amount of phosgene during the period, and then use nitrogen to drive off the excess phosgene and hydrogen chloride to obtain N-methylphenylcarbamoyl chloride dioxane solution;

[0023] (2) Chlorination reaction: Add 5g of the catalyst azobisisobutyronitrile to the aforementioned N-methylphenylcarbamoyl chloride dioxane solution, control the temperature of the photochemical kettle at 55°C, and pass 190g of chlorine gas into it to detect N- If the dichloromethylphenylcarbamoyl chloride is greater than 0.5%, the excess chlorine gas and by-product hydrogen chloride are purged with nitrogen to obtain the N-chloromethylphenylcarbamoyl chloride dioxane solution;

[0024]...

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PUM

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Abstract

The invention relates to a preparation method of buprofezin, which comprises the following steps of actinism, chlorination, synthesis and distillation crystallization. The actinism step employs dioxane or chloroform, the chlorination step employs dioxane or N-chloromethyl-N-phenyl carbamyl chloride as a solvent; and the synthesis step employs organic amine to participate in condensation. According to the invention, dioxane, chloroform or N-chloromethyl-N-phenyl carbamyl chloride are employed as the solvents, so that good dissolving performance is provided to the raw material, and the dioxane, chloroform or N-chloromethyl-N-phenyl carbamyl chloride has little solubility to HCL and is in favor of reaction, the production yield can reach as high as more than 82%; organic amine is employed for replacing ammonium bicarbonate as alkali for synthesis reaction, and can be recovered so that the discharge of ammonia nitrogen in waste water is reduced.

Description

Technical field [0001] The invention relates to a preparation method of Buprofezin. Background technique [0002] The chemical name of Buprofezin is 2-tert-butylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazine-4-one, the molecular formula is C16H23N3OS, and it is a heterocyclic ring. Insect chitin synthesis inhibitor, destroys the formation of new cuticles of insects, interferes with the normal growth and development of insects, and causes the death of insects. It has strong contact killing, stomach toxicity and permeability. Does not kill adults, but can reduce egg laying and hinder egg hatching. [0003] The existing production methods of buprofezin mainly include phosgene synthesis method and non-phosgene synthesis method. The phosgene synthesis method mainly involves the reaction of N-methylaniline with phosgene and chlorine to prepare intermediates. It reacts with the above-mentioned N-chloromethyl-N-phenylcarbamoyl chloride in the presence of a base to prepare buprofezin. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/34
CPCC07D285/34
Inventor 陆明若张中泽马志荣王卫华田庆海
Owner JIANGSU CHANGLONG AGROCHEM CO LTD
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