Preparation method of buprofezin

A technology of buprofezin and solution, which is applied in the field of preparation of buprofezin, can solve the problems of reducing total discharge, difficult treatment, environmental impact, etc., achieves the effect of reducing ammonia nitrogen wastewater and is conducive to environmental protection

Pending Publication Date: 2018-09-14
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method of Buprofezin, comprising the following steps:

[0026] Step 1): Preparation of tert-butyl isothiocyanate

[0027] Add sodium thiocyanate and water into the esterification kettle, stir to dissolve the sodium thiocyanate completely; then add tert-butanol and stir evenly; slowly raise the temperature to 80°C, add industrial hydrochloric acid dropwise while reflux, and return to reflux after the addition Keep warm for 2 hours under normal conditions, the molar ratio of sodium thiocyanate, tert-butanol and hydrochloric acid is 1:1:1.5; then cool down to 50°C, separate layers, and the acidic wastewater goes to the wastewater treatment tank, and the upper oil layer is added with an alkaline aqueous solution Washing, and then washing with water until the pH is 7.0, the light yellow oil layer liquid is returned to the reaction kettle equipped with a reflux water separation system, and the temperature is raised to carry out reflux with water until there is n...

Embodiment 2

[0034] A preparation method of Buprofezin, comprising the following steps:

[0035] Step 1): Preparation of tert-butyl isothiocyanate

[0036] Add sodium thiocyanate and water into the esterification kettle, stir to dissolve the sodium thiocyanate completely; then add tert-butanol and stir evenly; slowly raise the temperature to 70°C, add industrial hydrochloric acid dropwise while reflux, and return to reflux after the dropwise addition Keep warm for 3 hours under normal conditions, the molar ratio of sodium thiocyanate, tert-butanol and hydrochloric acid is 1:0.8:1.2; then cool down to 40°C, separate layers, acid waste water goes to waste water treatment tank, and alkaline aqueous solution is added to the upper oil layer Washing, and then washing with water until the pH is 6.8, the light yellow oil layer liquid is returned to the reaction kettle equipped with a reflux water separation system, and the temperature is raised to carry out reflux with water until there is no wate...

Embodiment 3

[0044] A preparation method of Buprofezin, comprising the following steps:

[0045] Step 1): Preparation of tert-butyl isothiocyanate

[0046] Add sodium thiocyanate and water into the esterification kettle, stir to dissolve the sodium thiocyanate completely; then add tert-butanol and stir evenly; slowly raise the temperature to 90°C, add industrial hydrochloric acid dropwise while reflux, and return to reflux after the dropwise addition Keep warm for 4 hours under normal conditions, the molar ratio of sodium thiocyanate, tert-butanol and hydrochloric acid is 1:0.8:1.2; then cool down to 70°C, separate layers, and the acidic waste water goes to the waste water treatment tank, and the upper oil layer is added with an alkaline aqueous solution Washing, and then washing with water until the pH is 7.2, the light yellow oil layer liquid is returned to the reaction kettle equipped with a reflux water separation system, and the temperature is raised to carry out reflux with water unt...

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PUM

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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 ...

Claims

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Application Information

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IPC IPC(8): C07D285/34
CPCC07D285/34
Inventor 朱学军姜育田唐素荣姚修宇
Owner JIANGSU ANPON ELECTROCHEM
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