Preparation method of buprofezin

Abstract

The invention provides a preparation method of buprofezin, comprising the steps of 1), adding sodium thiocyanate and water into an esterification kettle until dissolution; adding tertiary butanol andhydrochloric acid to obtain a mixed ester; allowing transposition and catalytic reaction to obtain t-butyl isothiocyanate; 2), adding the t-butyl isothiocyanate into chlorobenzene, stirring, dropwiseadding isopropyl amine to obtain 1-isopropyl-3-tert-butylthiourea solution; 3), adding N-methylaniline into chlorobenzene; introducing carbonyl chloride and chlorine gas in sequence to obtain N-chloromethyl-N-benzenecarbamoylchloride solution; 4), adding sodium bicarbonate into water, and adding the resultant into chlorobenzene; adding the 1-isopropyl-3-tert-butylthiourea solution; dropwise addingthe N-chloromethyl-N-benzenecarbamoylchloride solution, filtering, allowing layering, performing high-vacuum steaming to remove the chlorobenzene, crystallizing, centrifuging, and drying to obtain buprofezin. The substitutive average yield of the preparation process of buprofezin reaches 90% and above; the content of finished buprofezin reaches 98.0% and above; the preparation process is free ofammonia nitrogen wastewater.

Description

technical field [0001] The invention belongs to the technical field of chemical product synthesis, and in particular 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-thiadiazin-4-one, and its molecular formula is C16H23N3OS, which is a heterocyclic Insect chitin synthesis inhibitor, destroys the new cuticle formation of insects, interferes with the normal growth and development of insects, and causes the death of pests. It has strong contact and stomach poisoning effects and is permeable. Does not kill adults, but may reduce oviposition and hinder egg hatching. [0003] The preparation process of buprofezin in the prior art first uses ammonium thiocyanate and tert-butanol as raw materials to prepare tert-butanol isothiocyanate, through esterification, transposition, addition, chlorination and actinization, and finally through hydrogen carbonate Ammonia condensation ...

AI Technical Summary

Problems solved by technology

[0003] The preparation process of buprofezin in the prior art first uses ammonium thiocyanate and tert-butanol as raw materials to prepare tert-butanol isothiocyanate, through esterification, transposition, addition, chlorination and actinization, and finally through hydrogen carbonate Ammonia condensation produces buprofezin; due to the use of ammonium thiocyanate and ammonium bicarbonate, a large amount of ammonia nitrogen wastewater is produced in the production process of buprofezin, and because the wastewater is high in ammonia nitrogen, high COD, and high salt, it is difficult to treat. Production enterprises often use the method of diluting with clean water to discharge after reaching the standard, which does not reduce the total discharge and has an impact on the environment