Manufacturing method of proPiconazole

A production method and a technology for propiconazole, applied in the field of pesticides, can solve the problems of difficult dehydration, affect the refining yield, sticky materials, etc., and achieve the effects of reducing waste water discharge, reducing environmental pollution, and improving yield

Active Publication Date: 2011-10-26
山东潍坊双星农药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are following shortcoming in the production method that generally adopts at present: need carry out washing to remove impurity after bromination reaction, reversible reaction easily takes place during washing; The reaction time is long when synthesizing triazole potassium salt, is difficult for dehydration, and material is sticky; After a long time, the washed by-products after the reaction are not easy to recover, resulting in a large amount of waste water; when the product is purified, it is nitrated into salt, which is difficult to operate, and the product quality fluctuates greatly; partial oxidation occurs during high-vacuum rectification, which affects the refining yield

Method used

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  • Manufacturing method of proPiconazole

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Experimental program
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Effect test

Embodiment 1

[0053] According to the ratio of the amount of the substance 2,4-dichloroacetophenone: 1,2-pentanediol: the catalyst phosphomolybdic acid ratio of 1:1.07:0.02, the 2,4-dichloroacetophenone and 1, 2-Pentanediol is refluxed under the action of the catalyst phosphomolybdic acid for the cyclization reaction. At this time, the temperature is 86°C and the reaction time is 8 hours. After the cyclization reaction is completed, the catalyst phosphomolybdic acid is filtered and recovered for bromination reaction. The bromination reaction temperature is 35°C, and the bromine drop acceleration rate is 18Kg / h. After the bromination reaction is over, keep 0.3Mpa and stir for 1h, recover hydrogen bromide gas, and remove the solvent to obtain 2-bromomethyl-(2, 4-Dichlorophenyl)-4-propyl-1,3-dioxpentane. In the present invention, the synthesized cyclized product is first recovered to remove the catalyst phosphomolybdic acid, and then the bromination reaction is carried out. The rate can reach m...

Embodiment 2

[0056] According to the ratio of the amount of 2,4-dichloroacetophenone:1,2-pentanediol:catalyst phosphomolybdic acid is 1:1.13:0.06, the 2,4-dichloroacetophenone and 1, 2-Pentanediol is refluxed under the action of the catalyst phosphomolybdic acid to carry out the cyclization reaction. At this time, the temperature is 83~88℃, and the reaction time is 8 hours. After the cyclization reaction is completed, the catalyst phosphomolybdic acid is filtered and recovered for bromination reaction. The bromination reaction temperature is 36°C, and the bromine drop acceleration rate is 19Kg / h. After the bromination reaction is over, keep 0.4Mpa and stir for 1.5h, recover the hydrogen bromide gas, and remove the solvent to obtain 2-bromomethyl- (2,4-Dichlorophenyl)-4-propyl-1,3-dioxpentane. In the present invention, the synthesized cyclized product is first recovered to remove the catalyst phosphomolybdic acid, and then the bromination reaction is carried out. The yield of bromide can rea...

Embodiment 3

[0059] According to the ratio of the amount of 2,4-dichloroacetophenone:1,2-pentanediol:catalyst phosphotungstic acid of 1:1.20:0.1, combine 2,4-dichloroacetophenone and 1, 2-Pentanediol is refluxed under the action of the catalyst phosphotungstic acid for the cyclization reaction. At this time, the temperature is 85~89℃, and the reaction time is 4~8 hours. After the cyclization reaction is completed, the catalyst phosphomolybdic acid is filtered and recovered for bromine The bromination reaction temperature is 37°C, and the bromine drop acceleration rate is 20Kg / h. After the bromination reaction is over, keep 0.5Mpa and stir for 2h, recover hydrogen bromide gas, and remove the solvent to obtain 2-bromomethyl -(2,4-Dichlorophenyl)-4-propyl-1,3-dioxpentane. In the present invention, the synthesized cyclized product is first recovered to remove the catalyst phosphomolybdic acid, and then the bromination reaction is performed , The bromide yield can reach more than 98%wt, and the ...

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Abstract

The invention discloses a manufacturing method of proPiconazole. The manufacturing method comprises that 2,4-dichloroacetophenone and 1,2-pentanediol undergo a cyclization reaction, and then bromine and the reaction products of the cyclization reaction undergo a bromination reaction to form 2-bromomethyl-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane. The manufacturing method is characterized in that solid heteropolyacid catalysts are utilized in the cyclization reaction, and are filtered and recycled after the cyclization reaction is finished; then the bromination reaction is caused and the 2-bromomethyl-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane, 1,2,4-triazole and potassium carbonate undergo a condensation reaction to form the proPiconazole after the bromination reaction is finished. Through the manufacturing method, new impurities which can be introduced because catalysts take part in a bromination reaction are reduced. In the invention, because a potassium triazole preparation process, a condensation reaction process and a solvent removing process are carried out simultaneously during a condensation reaction, problems of long reaction time and adhesion of 1,2,4-triazole on a kettle are solved, and a reaction time and a production cost are reduced.

Description

Technical field [0001] The invention relates to the technical field of pesticides, in particular to a method for producing propiconazole technical. Background technique [0002] ProPiconazole is a tricloconazole systemic fungicide developed by Ciba-Geigy of Switzerland. The chemical name of propiconazole: cis-trans 1-2-(2, 4-dichloro) Phenyl)-4-propyl-1,3-dioxolane-2-methyl]-1H-1,2,4-triazole, which is a sterol demethylation agent with broad spectrum and systemic properties The appearance of the original drug is light yellow viscous silk liquid, boiling point (13.3Pa) 180°C, vapor pressure (ZOoC) 0.133mPa, refractive index 1.5468, specific gravity 1.279 / cm at 20°C 3 . The solubility in water is 110mg / L, and it is easily soluble in organic solvents. It is stable below 320℃, relatively stable to light, and the hydrolysis is not obvious. It is relatively stable in acidic and alkaline media and does not corrode metals. Storage stability for three years. Acute oral LD50 of the or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/06
CPCY02P20/584
Inventor 刘在成张春华范丰梅李金艳
Owner 山东潍坊双星农药有限公司
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