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Method for synthesizing thiazine ketone

A synthetic method, the technology of buprofezin, which is applied in the field of synthetic process of chemical products to achieve the effect of solving environmental protection problems

Active Publication Date: 2008-05-14
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of benzene, chlorinated benzene or its homologues to replace carbon tetrachloride in the production of buprofezin has not yet been reported in China.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 500L of benzene (430kg) was added to a 1000L reactor, stirred; 64.6kg of phosgene (content 80%, phosgene to N-methylaniline molar ratio of 1.4:1) was slowly introduced, and then 40kg of N-methylaniline was added dropwise. Base aniline, control the reaction temperature at 10-20°C, after the dripping, fill the phosgene until it is colorless and transparent. Add catalyst benzoyl peroxide then, pass into chlorine gas 35.2kg (the mol ratio of chlorine gas and N-methylphenylcarbamoyl chloride is 1.4: 1), sampling analysis after 1 hour, when chlorination conversion rate reaches 93% At ~97%, the chlorination reaction is complete. Connect a vacuum device to desolventize the chlorinated material under negative pressure. When the end point temperature is 100-110°C and the end point vacuum degree is ≥0.080MPa, the desolventization is completed, and 130.54kg of light yellow transparent liquid, N-chloromethyl The content of phenylcarbamoyl chloride is 45.6%, and the yield based on N...

Embodiment 2

[0023] Add 500L of chlorinated benzene (430kg) into a 1000L reactor, stir; slowly pass into phosgene 64.6kg (content 80%, phosgene and N-methylaniline molar ratio is 1.4:1), and then add dropwise 40kg of N-methylaniline, the reaction temperature is controlled at 50-60°C, after the dripping is completed, phosgene is replenished until it is colorless and transparent. Add catalyzer azobisisobutyronitrile then, pass into chlorine gas 35.2kg (the mol ratio of chlorine gas and N-methylphenylcarbamoyl chloride is 1.4: 1), sampling analysis after 1 hour, when chlorination conversion ratio reaches 93 % to 97%, the chlorination reaction is over. Connect a vacuum device to desolventize the chlorinated material under negative pressure. When the end point temperature is 120-130°C and the end point vacuum degree is ≥0.070MPa, the desolventization is completed, and 91.83kg of light yellow transparent liquid, N-chloromethyl The content of phenylcarbamoyl chloride is 65.8%, and the yield is 8...

Embodiment 3

[0025] Add 500L of chlorinated benzene (550kg) into a 1000L reactor and stir; slowly feed 74.3kg of phosgene (80% content, phosgene to N-methylaniline molar ratio of 1.3:1) and then dropwise add 50kgN -Methylaniline, the reaction temperature is controlled at 60-70°C, and after the dripping is completed, phosgene is replenished until it is colorless and transparent. Add catalyst benzoyl peroxide then, pass into chlorine gas 41kg (the mol ratio of chlorine gas and N-methylphenylcarbamoyl chloride is 1.3: 1), sampling analysis after 1 hour, when chlorination conversion rate reaches 93%~ At 97%, the chlorination reaction is over. Connect a vacuum device to desolventize the chlorinated material under negative pressure. When the end point temperature is 120-130°C and the end point vacuum degree is ≥0.075MPa, the desolventization is completed, and 160.82kg of light yellow transparent liquid is obtained, N-chloromethyl The content of phenylcarbamoyl chloride is 46.7%, and the yield b...

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PUM

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Abstract

The invention discloses a method for preparing buprofezin, which adopts benzene, chlorobenzene orhomologue as the solvent during the photochemical chlorination producing process of buprofezin to replace carbon tetrachloride used in the prior art. The phosgenation, chlorination and desolvation operations are performed on N-methylaniline to get the solution with the N-chloromethyl-phenyl-amido-formyl chloride. The invention has the advantages that average photochemical chlorination yield of the N-methylaniline is more than 80%, and buprofezin content in the finished product is more than 95.0%; benzene, chlorobenzene or homologue can entirely replace carbon tetrachloride to process industrial buprofezin production so as to avoid the environment pollution.

Description

technical field [0001] The invention relates to a synthesis process of chemical products, in particular to a synthesis method of Buprofezin. Background technique [0002] As the date of entry into force of the "Montreal Protocol" approaches, carbon tetrachloride will be banned, making it necessary to find alternatives for the carbon tetrachloride solvent used in the production of buprofezin. The use of benzene, chlorinated benzene or its homologues to replace carbon tetrachloride in the production of buprofezin has not yet been reported in China. Contents of the invention [0003] Purpose of the invention: the purpose of this invention is to provide a new synthetic method of buprofezin, in which a novel solvent is used to replace carbon tetrachloride in the production process of buprofezin, thereby solving the environmental protection problem. [0004] Technical solution: In order to achieve the above object, the synthetic method of Buprofezin of the present invention com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/34
Inventor 姜育田安礼如季玉祥王海超王俊生
Owner JIANGSU ANPON ELECTROCHEM
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