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Production method and equipment for reducing buprofezin impurities

A technology for thiazide and impurities, which is applied in the field of production methods and equipment for reducing thiazide impurities, can solve the problem of high impurity content of M291, and achieve the effects of improving yield, improving stirring stability and improving process methods.

Inactive Publication Date: 2021-05-25
JIANGSU ANPON ELECTROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem in the prior art that the content of M291 impurity in the original medicine of pibiling is relatively high, the present invention proposes a production method and equipment for reducing the impurity of buprofezin

Method used

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  • Production method and equipment for reducing buprofezin impurities
  • Production method and equipment for reducing buprofezin impurities
  • Production method and equipment for reducing buprofezin impurities

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0044] Put 115g (0.1mol) of tert-butyl isothiocyanate into the reaction kettle, raise the temperature to 50°C, increase the vacuum to -0.095Mpa, keep the vacuum stable, stir for 1 hour, and lose 0.5% of tert-butyl isothiocyanate;

[0045] Carbon disulfide in tert-butyl isothiocyanate was quantified by liquid chromatography, and the content was confirmed to be reduced to 0.08%;

[0046] The obtained tert-butyl isothiocyanate is added, cyclized and crystallized to obtain the original drug of buprofezin, and the content of M291 is 0.05%.

specific Embodiment 2

[0048] Put 115g (0.1mol) of tert-butyl isothiocyanate into the reaction kettle, raise the temperature to 70°C, increase the vacuum to -0.085Mpa, keep the vacuum stable, stir for 1 hour, and lose 0.5% of tert-butyl isothiocyanate;

[0049] Carbon disulfide in tert-butyl isothiocyanate was quantified by liquid chromatography, and the content was confirmed to be reduced to 0.03%;

[0050] The obtained tert-butyl isothiocyanate is added, cyclized and crystallized to obtain the original drug of buprofezin, and the content of M291 is 0.02%.

specific Embodiment 3

[0052] Put 115g (0.1mol) of tert-butyl isothiocyanate into the reaction kettle, raise the temperature to 80°C, increase the vacuum to -0.07Mpa, keep the vacuum stable, stir for 2 hours, the loss of tert-butyl isothiocyanate is 1.3%;

[0053] Carbon disulfide in tert-butyl isothiocyanate was quantified by liquid chromatography, and the content was confirmed to be reduced to 0.05%;

[0054] The obtained tert-butyl isothiocyanate is added, cyclized and crystallized to obtain the original drug of buprofezin, and the content of M291 is 0.02%.

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Abstract

The invention discloses equipment for reducing buprofezin impurities. The equipment comprises a kettle body, a power bearing, a stirring shaft and a supporting frame, wherein the power bearing comprises a motor, a driving shaft and a rotor, and the rotor is meshed with the kettle body. The invention also discloses a production method of the equipment for reducing the buprofezin impurities. The method comprises the following steps: adding tert-butyl isothiocyanate in a drying reaction kettle, heating, vacuumizing, and keeping the temperature and stirring in vacuum. The equipment is improved on the basis of the prior art, such that the stirring stability of the kettle body is effectively improved, the M291 impurity can be conveniently removed so as to improve the yield of the intermediate 1-isopropyl-3-tert-butylthiourea, the process method is improved, and the purposes of controlling the impurity M291 is achieved through the simple process operation, and therefore, the aim of conforming to production is fulfilled.

Description

technical field [0001] The invention relates to the technical field of pesticide production, in particular to a production method and equipment for reducing buprofezin impurities. Background technique [0002] Pudiling is a new type of insect growth regulator with high efficiency, long-lasting effect, strong selectivity and safety. It is currently the leading species for controlling rice planthoppers. Tert-butyl alcohol reacts in the presence of hydrochloric acid to obtain a mixture of tert-butyl thiocyanate and tert-butyl isocyanate (referred to as mixed ester), which is translocated to obtain tert-butyl isothiocyanate (abbreviated as isoester), and then reacted with isopropylamine Reaction to obtain 1-isopropyl-3-tert-butylthiourea (referred to as thiourea). In addition, react N-methyl-N-phenylcarbamoyl chloride with N-methylamine and phosgene, and then react with chlorine gas to obtain N-chloromethyl-N-phenylcarbamoyl chloride (chloride for short). Finally, the chloride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/18C07C335/08B01J19/00
CPCB01J19/18B01J19/0013C07C335/08
Inventor 姚修宇范锦龙杨玉坤李卫葛喜乐陈建国姜育田朱学军唐素荣万金方于同锋
Owner JIANGSU ANPON ELECTROCHEM
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