Production process for improving yield of hexazinone

A production process, the technology of hexazinone, applied in the field of hexazinone, can solve the problems of incomplete reaction of raw materials, low yield of raw material products of hexazinone, etc., achieve uncomplicated reaction principle, practical control of reaction process, and reduce residue Effect

Active Publication Date: 2021-02-26
ANHUI GUANGXIN AGROCHEM
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Problems solved by technology

[0005] The object of the present invention is to provide a kind of production technology that improves the yield of hexazinone, solves the problem that the reaction of raw materials in the production process existing in the technology is not complete, causes the yield of the raw material product of hexazinone to be low

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  • Production process for improving yield of hexazinone
  • Production process for improving yield of hexazinone
  • Production process for improving yield of hexazinone

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specific Embodiment

[0036] A production technique for improving the yield of hexazinone, specifically comprising the following steps:

[0037] Step S1, synthesis of methyl products: first add 1.1 parts by weight of cyanamide to the methylation kettle, add 64 parts by weight of liquid caustic soda and 3 parts by weight of ethyl chloroformate into the metering tank, and then open the methylation kettle After the temperature in the methylation kettle is lowered to 0°C, add liquid caustic soda and ethyl chloroformate dropwise to the methylation kettle, and control the temperature in the kettle to 2°C. After the addition of ethyl chloroformate is completed, Measure the pH value in the methylation kettle, when the pH value is stable at 8, stop dripping liquid caustic soda, and close the freezing valve of the methylation kettle; open the jacket water and steam inlet and outlet valves, Carry out heating, when heating up to 38 ℃, keep warm for 4h, stabilize the pH value in the methylation kettle by drippi...

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Abstract

The invention discloses a production process for improving the yield of hexazinone. The production process comprises the following steps: S1, generating ethyl cyanocarbamate by using cyanamide and ethyl chloroformate, and synthesizing a methyl substance from ethyl cyanocarbamate and dimethyl sulfate under the catalytic condition of a catalyst; S2, synthesizing a guanidine derivative from the methyl substance and dimethyl amine; S3, extracting the guanidine derivative for multiple times by using chloroform; S4, carrying out desolvation treatment on the guanidine derivative; S5, reacting the guanidine derivative with cyclohexyl isocyanate under the condition of taking methyl benzene as a solvent to synthesize a hexazinone intermediate; S6, carrying out cyclization reaction on the hexazinoneintermediate and sodium methoxide to prepare hexazinone, and carrying out water washing treatment; step S7, purifying and drying hexazinone to obtain a hexazinone prodrug product; the production process disclosed by the invention is easy for industrial production and strong in practicability, and solves the technical problem of low yield of hexazinone prodrug products in the prior art.

Description

technical field [0001] The invention belongs to the technical field of hexazinone, and in particular relates to a production process for improving the yield of hexazinone. Background technique [0002] Hexazinone is also known as Wilbur, Lincaojing, Feicaojing, Sentai; the chemical name is 3-cyclohexyl-6-dimethylamino-1-methyl-1,3,5-triazine-2, 4-Diketone, a colorless, odorless crystalline solid, is a systemic selective, post-emergent triazepine herbicide. [0003] Hexazinone is mainly used in the maintenance and opening of forest fire breaks, tending young forests, forest transformation, and weeding and irrigation along railways, highways, airports, warehouses, and docks, and has special effects on the prevention of "Canada solidago". This product is extremely lethal to forest weeds, shrubs, vines and other plants. It can be absorbed by the stems and leaves of plants, conduct conduction through the xylem inside the plants, and directly interfere with the photosynthesis of ...

Claims

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Application Information

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IPC IPC(8): C07D251/46
CPCC07D251/46
Inventor 李行操晶晶刘长庆朱光文胡梓杨李波潘荣欢邵辉望李健庞有顺程伟家
Owner ANHUI GUANGXIN AGROCHEM
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