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Synthesis method of trifloxystrobin

A synthetic method, the technology of trifloxystrobin, which is applied in the field of trifloxystrobin synthesis, can solve the problems of difficulty in industrial production, incomplete process, and difficulty in obtaining raw materials, and achieve the effects of improving product quality, avoiding cross-contamination, and reducing side reactions

Active Publication Date: 2015-04-15
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many reports on the synthesis literature of trifloxystrobin, the route is basically the same, but the alkali and solvent used are different, but so far, there are still many problems in the preparation process, raw materials are difficult to obtain, the process is incomplete, and the yield is low. bring great difficulty

Method used

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  • Synthesis method of trifloxystrobin
  • Synthesis method of trifloxystrobin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add compound I (21.0 g, 0.100 mol, 97%) and sodium hydroxide (4.2 g, 0.100 mol, 95%) to the reaction flask equipped with a stirrer, water separator, condenser and thermometer after nitrogen replacement and toluene (45.0g), start stirring, heat to reflux to divide water, reflux for 4 hours, stop heating, cool down to room temperature, dissolve compound II (31.6g, 0.105mol, 95%) in toluene (20.0g ), the toluene solution of compound II was added dropwise to the above reaction solution, and added dropwise for 0.5 hours, kept at 30°C for 3 hours, then sampled and analyzed, and after the reaction was completed, the reaction was processed. Add water (50g) to the reaction solution, stir for 10 minutes, let stand, separate layers, wash the organic phase with water (wash twice, 50ml each time), the pH of the water after washing is 6, the organic phase cools down and crystallizes, and keep warm at 20°C for 1 Hours, part of the solid precipitated, kept at 10°C for 2 hours, kept at ...

Embodiment 2

[0022] Add compound I (21.0g, 0.100mol, 97%) and potassium hydroxide (6.2g, 0.100mol, 90%) to the reaction flask equipped with a stirrer, water separator, condenser and thermometer after nitrogen replacement and benzene (45.0g), start stirring, heat to reflux to divide water, reflux for 4 hours, stop heating, cool down to room temperature, dissolve compound II (31.6g, 0.105mol, 95%) in toluene (20.0g ), the toluene solution of compound II was added dropwise to the above reaction solution, and added dropwise for 0.5 hours, kept at 30°C for 3 hours, then sampled and analyzed, and after the reaction was completed, the reaction was processed. Add water (50g) to the reaction solution, stir for 10 minutes, let stand, separate layers, wash the organic phase with water (wash twice, 50ml each time), the pH of the water after washing is 6.5, the organic phase cools down and crystallizes, and keep warm at 20°C for 1 Hours, part of the solid precipitated, kept at 10°C for 2 hours, kept at...

Embodiment 3

[0024] Add compound I (21.0 g, 0.100 mol, 97%) and sodium hydroxide (4.2 g, 0.100 mol, 95%) to the reaction flask equipped with a stirrer, water separator, condenser and thermometer after nitrogen replacement and cyclohexane (45.0g), start stirring, heat to reflux to divide water, reflux for 4 hours, stop heating, cool down to room temperature, dissolve compound II (31.6g, 0.105mol, 95%) in cyclohexane Alkanes (20.0g), the cyclohexane solution of compound II was added dropwise to the above reaction solution, added dropwise for 0.5 hours, kept at 30°C for 3 hours, then sampled and analyzed, after the reaction was completed, the reaction was processed. Add water (50g) to the reaction solution, stir for 10 minutes, let stand, separate layers, wash the organic phase with water (wash twice, 50ml each time), the pH of the water after washing is 7.5, the organic phase cools down and crystallizes, and keep warm at 20°C for 1 Hours, part of the solid precipitated, kept at 10°C for 2 ho...

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Abstract

The invention relates to a synthesis method of trifloxystrobin. A reaction process of the synthesis method includes water diversion treatment. By virtue of a water carrying process, the influence of water formed in the reaction on the reaction is effectively avoided, thereby reducing side reaction, and improving product yield and product quality. According to the synthesis method, a reaction liquid solvent is directly used for crystallization after the reaction so as to avoid change of a crystallization solvent and to avoid cross infection of the solvents, thus further enhancing product quality.

Description

Technical field [0001] The invention relates to a synthesis method of trifloxystrobin. Background technique [0002] Trifloxystrobin broad-spectrum fungicides are a new class of fluorinated fungicides successfully developed from the natural product Strobilurins as lead fungicide compounds. It has the characteristics of high efficiency, broad spectrum, protection, treatment, eradication, penetration, systemic absorption, activity, resistance to rain erosion, and long lasting effect. It is effective against strains resistant to 1,4-demethylase inhibitors, benzamides, dicarboxylamines and benzimidazole. It has no cross-resistance with currently existing fungicides and is effective against almost all fungi. It has good activity against diseases of various classes (Ascomycetes, Basidiomycetes, Oomycetes and Deuteromycetes) such as powdery mildew, rust, blight, net spot, downy mildew, rice blast, etc. In addition to having special effects on powdery mildew and leaf spot, it also...

Claims

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Application Information

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IPC IPC(8): C07C251/60C07C249/04
Inventor 何永利丁菲鞠晓东蔡军义
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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