Manufacturing method of proPiconazole

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

Active Publication Date: 2014-04-02
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 substance amount 2,4-dichloroacetophenone: 1,2-pentanediol: the ratio of catalyst phosphomolybdic acid is 1:1.07:0.02, 2,4-dichloroacetophenone and 1, 2-Pentanediol was refluxed under the action of catalyst phosphomolybdic acid to carry out cyclization reaction. At this time, the temperature was 86° C., and the reaction time was 8 hours. After the cyclization reaction was finished, the bromination reaction was carried out after the catalyst phosphomolybdic acid was recovered by filtration. Said bromination reaction temperature is 35 ℃, and bromine drip rate is 18Kg / h, after bromination reaction finishes, keep 0.3Mpa and stir 1h, reclaim hydrogen bromide gas, desolventize obtains 2-bromomethyl-(2, 4-dichlorophenyl)-4-propyl group-1,3-dioxolane, in the present invention, first reclaims and removes catalyst phosphomolybdic acid to the synthesized cyclized product, then carries out bromination reaction, and bromide collects The rate can reach more ...

Embodiment 2

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

Embodiment 3

[0059] According to the ratio of substance amount 2,4-dichloroacetophenone: 1,2-pentanediol: the ratio of catalyst phosphotungstic acid is 1:1.20:0.1, 2,4-dichloroacetophenone and 1, 2-Pentanediol is refluxed under the action of catalyst phosphotungstic acid for cyclization reaction. At this time, the temperature is 85-89°C and the reaction time is 4-8 hours. bromination reaction, the bromination reaction temperature is 37 ° C, and the bromine drop rate is 20Kg / h, after the bromination reaction is completed, keep stirring at 0.5Mpa for 2h, recover hydrogen bromide gas, and remove the solvent to obtain 2-bromomethyl -(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane, in the present invention, first recover and remove catalyst phosphomolybdic acid to the synthesized cyclized product, then carry out bromination reaction , the yield of bromide can reach more than 98%wt, and the mass content of bromide is more than 98%, reducing the monobromide and dibromide of ketone due to the re-decom...

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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 production method of the original drug of propiconazole. Background technique [0002] Propiconazole (proPiconazole) is a kind of cyclobutanazole systemic fungicide developed by Swiss Ciba-Geigy Corporation, the chemical name of propiconazole: cis-trans 1-"2-(2,4-dichloro Phenyl)-4-propyl-1,3-dioxolane-2-ylmethyl]-1H-1,2,4-triazole is a sterol demethylation agent with broad-spectrum and systemic properties The appearance of the original drug is a light yellow viscose liquid, with a boiling point (13.3Pa) of 180°C, a vapor pressure (ZOoC) of 0.133mPa, a refractive index of 1.5468, and a specific gravity of 1.279 / cm at 20°C 3 . The solubility in water is 110mg / L, easily soluble in organic solvents. Stable below 320°C, relatively stable to light, and not obvious in hydrolysis. It is relatively stable in acidic and alkaline media and does not corrode metals. Storage stabili...

Claims

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Application Information

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Patent Type & Authority Patents(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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