Novel method for synthesizing fungicide tebuconazole

The technology of a tebuconazole and a new method is applied in the new field of synthesizing the fungicide tebuconazole, can solve problems such as unsatisfactory, and achieve the effects of suppressing side reactions, reducing the generation of impurities, and improving the reaction yield

Inactive Publication Date: 2008-02-27
SHANGHAI SHENGNONG PESTICIDE
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The highest yield of the above patents is only 83.4%, obviously unsatisfactory

Method used

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  • Novel method for synthesizing fungicide tebuconazole
  • Novel method for synthesizing fungicide tebuconazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0011] Pump 50kg N, N-dimethyldecylamide and 600kg epoxy compound into a dry and clean 2000L glass-lined reactor. Open the inlet hole and drop in 265kg potassium hydroxide and 225kg triazole. Close the inlet hole, raise the temperature to 80° C., and then keep it warm at this temperature for 15 hours. Sampling and analysis shows that the peak of the raw material is less than 0.5% as the end point of the reaction. After the reaction is over, add cold water to full while it is hot, stir until the crystals are precipitated, turn on cold water to cool down for about 3 hours, put the material into the suction filter, filter with suction, wash the filter cake with water, drain it and wait for refinement.

[0012] Put the above crude product into a 5000L refining kettle, add 1400kg of n-hexane and 100kg of methanol to heat up and flow for 0.5 hours, cool down to 10°C, keep this temperature for 1 hour, discharge the material and suction filter, recover the n-hexane-methanol mixed solv...

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Abstract

The invention discloses a tebuconazole as high-efficiency triazole bactericide, which is characterized by the following: adopting one solvent with catalytic action to improve the receiving rate over 90%; using one composite solvent to recrystallize; making the content of tebuconazole over 97%; realizing industrialization effectively.

Description

technical field [0001] Pesticide synthesis. Background technique [0002] Tebuconazole is a highly effective triazole fungicide. Its synthesis is generally obtained by reacting epoxy compounds and 1,2,4-triazole in the presence of a solvent and refining it. For example, in U.S.4.723.984, epoxy compound, triazole, and ethanol were reacted at 150° C. in an autoclave for 20 hours. The reaction mixture was cooled, degassed, evaporated to remove ethanol, crystallized from ether, and then recrystallized from acetonitrile to obtain the product, m.p.139-141°C, yield 77%. [0003] [0004] U.S.4.929.735 uses epoxy compound and 1,2,4-triazole in the presence of dimethyl sulfoxide solvent and sodium carbonate, reacted at 110° C. for 4 hours, and the product yield was only 42%. [0005] DE 3.733.754 used epoxy compound and 1,2,4-triazole in the presence of tert-butanol solvent and potassium hydroxide for azeotropic dehydration at 133°C for 4 hours to obtain a product yield of 83.4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/08
Inventor 董建生张振国施顺发程志明
Owner SHANGHAI SHENGNONG PESTICIDE
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