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A kind of high-purity difenoconazole synthesis method

A technology of difenoconazole and a synthesis method, applied in directions such as organic chemistry, can solve the problems such as large influence of color of fine difenoconazole, large influence of particle size, difficult separation, etc., to improve product content and appearance The effect of high quality, high yield and high quality

Active Publication Date: 2022-03-25
JIANGSU HEBEN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The biggest problem with this route is that when intermediate 1 prepares intermediate 2, dibrominated side reactions are prone to occur, and the side reactions are as follows:
[0011] The by-products of hydrolysis and difenoconazole are easy to form a eutectic, which is difficult to separate, and has a great impact on the drying section, and is easy to form larger particles. Even if difenoconazole is purified by recrystallization , a small amount of hydrolysis by-products still have a greater impact on the particle size of difenoconazole fine; while dibrominated by-products have a greater impact on the color of difenoconazole fine, making it light gray in color and affecting the appearance

Method used

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  • A kind of high-purity difenoconazole synthesis method

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Effect test

Embodiment 1

[0038] 1) Put 75g 99.7% 3,4'-dichlorodiphenyl ether, 50g 99.5% anhydrous aluminum trichloride, 100g dichloroethane in an empty reactor, and control the temperature at 10-50 ℃, then add 30g99.5% acetyl chloride dropwise, drop acetyl chloride in 1-4 hours, keep warm for 3-4 hours after dropping, the reaction is completed, drop the reaction solution into 200g water at 10-50℃, after dropping, stir for 15 Minutes, phase separation, the lower floor material is the dichloroethane solution of intermediate I;

[0039] 2) In an empty reactor, put the dichloroethane solution of intermediate I prepared in step 1), 1g of concentrated sulfuric acid, heat up to reflux, and add 30g of propylene glycol dropwise under reflux, and drop it in 1-3 hours After dripping, reflux and keep warm for 1-3 hours, the reaction is completed, add 200g of water, separate the phases, and obtain the dichloroethane solution of intermediate II;

[0040] 3) In an empty reactor, put 30g98% 1,2,4-triazole, 19.5g90% ...

Embodiment 2

[0044] 1) Put 75.00g of 99.7% 3,4'-dichlorodiphenyl ether, 48.34g of 99.5% anhydrous aluminum trichloride, and 97.50g of dichloroethane into an empty reactor, and control the temperature at 10-50°C, then add 29.78g 99.5% acetyl chloride dropwise, drop acetyl chloride in 1-4 hours, keep warm for 3-4 hours after dropping, the reaction is complete, drop the reaction solution into 187.50g water at 10-50°C, drop After finishing, stir for 15 minutes, phase separation, the lower floor material is the dichloroethane solution of intermediate I;

[0045]2) In an empty reactor, put the dichloroethane solution of intermediate I prepared in step 1), 0.49g sodium bisulfate, heat up to reflux, and add 29.80g propylene glycol dropwise under reflux, 1-3 After 1 hour of dripping, reflux and keep warm for 1-3 hours after dripping, the reaction is completed, add 187.50g of water, separate phases, and obtain the dichloroethane solution of intermediate II;

[0046] 3) Put 28.72g of 98% 1,2,4-triaz...

Embodiment 3

[0050] 1) Put 76.00g of 99.7% 3,4'-dichlorodiphenyl ether, 54.71g of 99.5% anhydrous aluminum trichloride, and 150.00g of dichloroethane into an empty reactor, and control the temperature at 10-50°C, then add 37.13g99.5% acetyl chloride dropwise, drop acetyl chloride in 1-4 hours, keep warm for 3-4 hours after dropping, the reaction is complete, drop the reaction solution into 375.00g water at 10-50°C, drop After finishing, stir for 15 minutes, phase separation, the lower floor material is the dichloroethane solution of intermediate I;

[0051] 2) In an empty reactor, put the dichloroethane solution of intermediate I prepared in step 1), 9.75g sodium p-toluenesulfonate, heat up to reflux, and drop 42.91g propylene glycol under reflux state, 1 After dropping in 3 hours, keep it under reflux for 1-3 hours, the reaction is complete, add 375.00 g of water, separate the phases, and obtain the dichloroethane solution of intermediate II;

[0052] 3) Put 35.85g of 98% 1,2,4-triazole,...

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Abstract

The invention discloses a method for synthesizing high-purity difenoconazole. The synthetic route is as follows: 1) intermediate I is prepared by acylation of 3,4'-dichlorodiphenyl ether; 2) cyclization reaction of intermediate I Preparation of intermediate II; 3) Bromination of 1,2,4-triazole to produce 1,2,4-triazole bromide; 4) Intermediate II and 1,2,4-triazole bromide Bromination reaction to obtain intermediate III and triazole, intermediate III and 1,2,4-triazole are condensed under the action of potassium hydroxide to obtain crude difenoconazole; 5) difenoconazole The crude product is refined to obtain difenoconazole fine product. The invention has the advantages of low cost, high quality and high yield, almost no dibromination and hydrolysis by-products, and improves the product content and appearance quality of the fine difenoconazole.

Description

technical field [0001] The invention relates to the technical field of pesticide technical preparation, in particular to a method for synthesizing high-purity difenoconazole. Background technique [0002] Difenoconazole has a wide bactericidal spectrum and is relatively safe among triazole fungicides. It is widely used in fruit trees, vegetables and other crops to effectively prevent and control scab, black pox, white rot, spotted leaf disease, and powdery mildew. disease, brown spot, rust, stripe rust, head blight, etc. [0003] At present, there are two main routes for the industrial production of difenoconazole: [0004] Route 1: The raw material 3,4'-dichlorodiphenyl ether is acylated, cyclized, brominated, condensed, and refined to prepare difenoconazole. [0005] ; [0006] The biggest problem with this route is that when intermediate 2 is used to prepare intermediate 3, side reactions of ketal hydrolysis are prone to occur, and the side reactions are as follows: ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/06
CPCC07D405/06
Inventor 冯魏陈华贾利华邓桂元陆健邢燕
Owner JIANGSU HEBEN BIOCHEM
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