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Synthesis technology for propiconazole

A synthesis process, the technology of propiconazole, which is applied in the field of synthesis process of propiconazole, can solve the problems such as hydrogen bromide pollution, and achieve the effect of high product purity and simple process

Pending Publication Date: 2019-06-14
CHANGSHA XINBEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the deficiencies in the prior art, the invention provides a synthesis process of propiconazole, which has a high utilization rate of bromine atoms, does not produce tail gas hydrogen bromide, solves the problem of hydrogen bromide pollution, and improves product purity. Reduced production costs and high industrial production value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 300 milliliters of dichloromethane into a 1000 milliliter four-neck flask equipped with a stirrer, thermometer, condenser and constant pressure titration funnel, and add 189 grams of 2,4-dichloroacetophenone and 120 milliliters of 27.5% Hydrogen peroxide, 15 grams of sodium percarbonate, and then slowly add 80 grams of bromine dropwise at room temperature, cooling is required during the dropping process, and the temperature of the material is controlled not to exceed 40°C. After the bromine addition is completed, keep warm at 40°C-45°C for 1-8 hours, take a sample every 30 minutes, and detect it with liquid chromatography. After the conversion rate of the raw material reaches 99.5%, add 20 milliliters of saturated sodium carbonate aqueous solution to The reaction solution became colorless. Stirring was stopped and the layers were allowed to stand, the aqueous phase was extracted twice with 100 milliliters of dichloromethane, the combined organic phase was washed twi...

Embodiment 2

[0029] Add 400 milliliters of dichloroethane into a 1000 milliliter four-necked flask equipped with a stirrer, thermometer, condenser and constant pressure titration funnel, and add 189 grams of 2,4-dichloroacetophenone and 150 milliliters of 27.5% Hydrogen peroxide, 15 grams of sodium percarbonate, then slowly add 80 grams of bromine dropwise at room temperature, cooling is required during the dropping process, and the temperature of the material is controlled not to exceed 40°C. After the bromine addition is completed, keep warm at 40°C-45°C for 1-8 hours, take a sample every 30 minutes, and detect it with liquid chromatography. After the conversion rate of the raw material reaches 99.5%, add 20 ml of hydroxylamine hydrochloride aqueous solution until the reaction The liquid is colorless. Stop stirring and let stand to separate the layers. The aqueous phase was extracted twice with 100 ml of dichloroethane, and the combined organic phase was washed twice with 200 ml of satur...

Embodiment 3

[0033]Add 300 milliliters of acetonitrile into a 1000 milliliter four-necked flask equipped with a stirrer, thermometer, condenser and constant pressure titration funnel, add 189 grams of 2,4-dichloroacetophenone and 120 milliliters of 27.5% hydrogen peroxide successively under stirring, 15 grams of sodium percarbonate, and then slowly add 80 grams of bromine dropwise at room temperature, cooling is required during the dropping process, and the temperature of the material is controlled not to exceed 40°C. After the addition of bromine, keep it warm at 40°C-45°C for 1-8 hours, take a sample every 30 minutes, and detect it with liquid chromatography. After the conversion rate of the raw material reaches 99.5%, add 20 ml of 80% hydrazine hydrate solution , until the reaction solution is colorless. Stop stirring and let stand to separate the layers. The water phase was extracted twice with 100 ml of acetonitrile respectively. The combined organic phase was washed twice with 200 ml...

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PUM

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Abstract

The invention discloses a synthesis technology for propiconazole. The synthesis technology comprises the following steps: 1) successively adding an organic solvent, 2,4-dichlorophenone, hydrogen peroxide and a catalyst into a reaction tank and dropwise adding liquid bromine; 2) keeping temperature at 40-45 DEG C for 1-8 hours and adding a reducing agent; 3) drying with magnesium sulfate and performing reduced pressure distillation; 4) cooling, separating and drying, thereby acquiring alpha-2,4-dichlorophenone; 5) adding methylbenzene, alpha-2,4-dichlorophenone, 1,2-pentanediol and p-toluene sulfonic acid into the reaction tank, heating till reflux reaction for 4-8 hours, and performing reduced pressure distillation, thereby acquiring 2-(2,4-dichlorophenyl)-2-bromine methyl-4-propyl-1,3-dioxolame; 6) adding dimethyl sulfoxide, catalyst, 1,2,4-triazole potassium and 2-(2,4-dichlorophenyl)-2-bromine methyl-4-propyl-1,3-dioxolame into the reaction tank, keeping temperature at 140 DEG C for5-10 hours, cooling, filtering, performing reduced pressure distillation, generating a salt with nitric acid, acidizing and neutralizing, performing reduced pressure distillation and purifying, thereby acquiring propiconazole. The synthesis technology disclosed by the invention is simple, environment-friendly and high in product purity.

Description

technical field [0001] The invention relates to fine chemical technology, in particular to a synthesis process of propiconazole. Background technique [0002] Propiconazole is a new broad-spectrum fungicide of systemic triazoles with dual functions of treatment and protection, which can be absorbed by the roots, stems and leaves of plants, and can quickly enter the plant Conduct upward transmission to prevent and control diseases caused by Ascomycetes, Basidiomycetes and Deuteromycetes, especially for wheat take-all, powdery mildew, rust, root rot, rice bakanae disease, sheath blight, banana leaf spot and other diseases Special effect, can effectively control the diseases caused by most higher fungi. Its dispersant is used to prevent and control diseases of vegetables, melons and fruits in greenhouses. It is safe and convenient, and its effective period is as long as 3 months. It also has obvious effects on the storage and preservation of fruits, especially citrus, apple a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/06
Inventor 刘建李刚
Owner CHANGSHA XINBEN CHEM