Production process for synthesizing tricyclazole by using solid super acid

A solid super acid and production process technology, applied in the field of pesticides, can solve the problems of large environmental pollution, low utilization rate of formic acid, and low recovery rate, and achieve the effects of reducing pollution, eliminating recovery and purification processes, and improving utilization rate.

Active Publication Date: 2018-12-07
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the formic acid utilization rate of this patent is low, and recovery rate is low, and environmental pollution is big
[0007] Therefore, in order to overcome the shortcoming and deficiency of the low utilization rate of formic acid existing in the prior art, it is necessary to provide a new and efficient production process for the synthesis of tricyclazole

Method used

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  • Production process for synthesizing tricyclazole by using solid super acid

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Experimental program
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Effect test

Embodiment 1

[0028] A production process for synthesizing tricyclazole using solid superacid, using intermediate 4-methyl-2-hydrazinobenzothiazole as raw material, formic acid as cyclizing agent, chlorobenzene as solvent, and solid superacid as catalyst to synthesize tricyclazole Azole; the solid superacid is perfluorosulfonic acid resin; 179kg of 4-methyl-2-hydrazinobenzothiazole, 537kg of chlorobenzene, 172.5kg of 40% formic acid, and 8.95kg of solid superacid.

[0029] The production technique of using solid superacid to synthesize tricyclazole comprises the following steps:

[0030] Step S1, mixing the 4-methyl-2-hydrazinobenzothiazole with the chlorobenzene, then adding the formic acid, and raising the temperature to reflux until the 4-methyl-2-hydrazinobenzothiazole is completely converted Forming an oxime-based intermediate; wherein, the heating temperature for heating and refluxing is 136°C; the time for heating and refluxing is 0.5h;

[0031] Step S2, adding the solid superacid t...

Embodiment 2

[0033] A production process for synthesizing tricyclazole using solid superacid, using intermediate 4-methyl-2-hydrazinobenzothiazole as raw material, formic acid as cyclizing agent, chlorobenzene as solvent, and solid superacid as catalyst to synthesize tricyclazole Azole; the solid superacid is perfluorosulfonic acid resin; 179kg of 4-methyl-2-hydrazinobenzothiazole, 626.5kg of chlorobenzene, 53.67kg of 90% formic acid, and 17.9kg of solid superacid.

[0034] The production technique of using solid superacid to synthesize tricyclazole comprises the following steps:

[0035] Step S1, mixing the 4-methyl-2-hydrazinobenzothiazole with the chlorobenzene, then adding the formic acid, and raising the temperature to reflux until the 4-methyl-2-hydrazinobenzothiazole is completely converted Forming an oxime-based intermediate; wherein, the heating temperature for heating and refluxing is 139°C; the time for heating and refluxing is 2h;

[0036] In step S2, add the solid superacid t...

Embodiment 3

[0038] A production process for synthesizing tricyclazole using solid superacid, using intermediate 4-methyl-2-hydrazinobenzothiazole as raw material, formic acid as cyclizing agent, chlorobenzene as solvent, and solid superacid as catalyst to synthesize tricyclazole Azole; the solid superacid is perfluorosulfonic acid resin; 179kg of 4-methyl-2-hydrazinobenzothiazole, 600kg of chlorobenzene, 85.43kg of 70% formic acid, and 12kg of solid superacid.

[0039] The production technique of using solid superacid to synthesize tricyclazole comprises the following steps:

[0040] Step S1, mixing the 4-methyl-2-hydrazinobenzothiazole with the chlorobenzene, then adding the formic acid, and raising the temperature to reflux until the 4-methyl-2-hydrazinobenzothiazole is completely converted Forming an oxime-based intermediate; wherein, the heating temperature for heating and refluxing is 138°C; the time for heating and refluxing is 1.5h;

[0041]In step S2, add the solid superacid to r...

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Abstract

The invention discloses a production process for synthesizing tricyclazole by using a solid super acid. The process takes an intermediate 4-methyl-2-hydrazinobenzothiazole as a raw material, formic acid as a ring-closing agent, chlorobenzene as a solvent, and the solid super acid as a catalyst for synthesizing the tricyclazole, wherein the solid super acid is perfluorosulfonic acid resin. The process comprises the following steps: mixing 4-methyl-2-hydrazinobenzothiazole with chlorobenzene, then adding formic acid, conducting heating for refluxing until the 4-methyl-2-hydrazinobenzothiazole iscompletely converted into an oximido intermediate; then adding the solid super acid, conducting refluxing for dehydrating, when the reaction reaches the end point, filtering out the solid super acidwhile the system is hot, then removing the solvent from the mother liquor, adding water for crystallization, conducting cooling, filtering, water washing and drying to obtain the tricyclazole. The production process disclosed by the invention creatively introduces the solid super acid as the catalyst, and uses a slight excess of formic acid to efficiently synthesize the tricyclazole, thereby increasing the utilization rate of formic acid from 10% to 70% or more, and greatly improving the utilization rate of formic acid.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a production process for synthesizing tricyclazole with a solid superacid. Background technique [0002] Tricyclazole is a special fungicide for the control of rice blast. It belongs to the thiazole tricyclazole. It has the characteristics of high efficiency, long-lasting effect and less frequency of use in the field control of rice blast. Its bactericidal mechanism is mainly to inhibit the formation of episporium melanin, thereby inhibiting spore germination and epispora formation, preventing the invasion of pathogens and reducing the production of spores of blast fungus. [0003] There are many synthetic routes for the synthesis of tricyclazole. At present, the vast majority of production units use o-toluidine as the starting material to prepare through the synthetic route of condensation, cyclization, substitution, and secondary cyclization. In the last step In the reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D513/04
CPCC07D513/04
Inventor 徐齐恩王进潘光飞陈华戴光炳陈云南彭彩群李成斌
Owner 浙江禾本科技股份有限公司
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