Preparation method of high-purity pyrimethanil and equipment used for preparing high-purity pyrimethanil

A pyrimethamine, high-purity technology, applied in the field of pesticide preparation, can solve the problems that it is difficult to meet the requirements, the original drug product cannot meet the requirements, etc., and achieves the effects of reducing the solubility, reducing the generation of acetone, and reducing hydrolysis.

Active Publication Date: 2015-05-13
利民化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The original drug products made by traditional technology cannot meet the requirements, and even the refined method is diff...

Method used

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  • Preparation method of high-purity pyrimethanil and equipment used for preparing high-purity pyrimethanil
  • Preparation method of high-purity pyrimethanil and equipment used for preparing high-purity pyrimethanil
  • Preparation method of high-purity pyrimethanil and equipment used for preparing high-purity pyrimethanil

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Experimental program
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Embodiment 1

[0037] in each batch

[0038] Aniline: 16.4Kmol (99%)

[0039] Hydrochloric acid: 15.7Kmol (30%)

[0040] Cyanamide: 16.6Kmol (30%)

[0041] Sodium carbonate: 16.4Kmol (99%)

[0042] Acetylacetone: 19.7Kmol (99%)

[0043] Feed nitrogen into the reaction kettle, replace the oxygen in the reaction kettle (oxygen content ≤ 2%), add 16.4Kmol aniline to the reaction kettle, start stirring after the aniline is added, raise the temperature to 50°C, and drop Add 11.8Kmol of hydrochloric acid once, control the reaction temperature at 50-60°C, and finish the dropwise addition in 1 hour. After the dropwise addition, raise the temperature to 80°C, start dropping 8.3Kmol of cyanamide once, and control the temperature at 80-85°C. Cyanamide, control the temperature at 85-90°C. After the dropwise addition, raise the temperature to 100°C, and keep the temperature for 5 hours; after the heat preservation reaction, cool to 60°C, put the prepared saturated sodium carbonate solution (50°C) i...

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PUM

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Abstract

The invention discloses a preparation method of high-purity pyrimethanil. The method comprises the following steps: by taking phenylamine, hydrochloric acid, hydrogen cyanamide, sodium carbonate and acetylacetone as raw materials, charging nitrogen to protect during the whole process, adding hydrochloric acid and hydrogen cyanamide twice respectively, and strictly controlling the molar amount of hydrochloric acid to synthesize phenylguanidine carbonate; carrying out cyclization dehydration on the obtained phenylguanidine carbonate and acetyl benzophenone to prepare pyrimethanil. The invention further discloses equipment for preparing high-purity pyrimethanil by using the preparation method of high-purity pyrimethanil.

Description

technical field [0001] The invention relates to the field of pesticide preparation, in particular to a preparation process and equipment for the fungicide pyrimethanil. Background technique [0002] Pyrimethanil is a pyrimidine amine fungicide developed by German Agford Company. Its chemical name is N-(4,6-dimethylpyrimidine-ethyl)aniline. It is mainly used to prevent gray mold and scab of various crops. It is an excellent broad-spectrum, high-efficiency, low-toxicity, systemic fungicide, and has achieved remarkable results in crop sterilization and yield increase. Therefore, pyrimethanil is the first choice of fungicides in countries all over the world. [0003] The original drug is colorless crystal or white crystal, soluble in organic solvents, slightly soluble in water, solubility in water at room temperature (25°C) is 0.12Kg / L, melting point at 25°C is 96.3°C (pure product), vapor pressure 2.2×10 -3 Pa (25°C), stable under weak acid and weak alkaline conditions, speci...

Claims

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Application Information

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IPC IPC(8): C07D239/42
CPCC07D239/42
Inventor 孙敬权唐启举
Owner 利民化学有限责任公司
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