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A kind of production method of dimethomorph

A production method, dimethomorph technology, applied in the field of dimethomorph production, can solve the problems of death, dimethomorph conversion rate and purity reduction, catalytic effect reduction, etc., to achieve the effect of improving conversion rate and purity

Active Publication Date: 2021-04-09
江苏恒隆作物保护有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In a broad sense, pesticides refer to the prevention, elimination or control of diseases, insects, weeds and other harmful organisms that endanger agriculture and forestry by purposefully regulating, controlling and affecting the metabolism, growth, development and reproduction of harmful organisms; In a narrow sense, it refers to a class of drugs used to kill insects, fungicides or harmful weeds in order to ensure and promote the growth of plants and crops in agricultural production. Dimethomorph is a systemic therapeutic low-toxic bactericidal Its mechanism of action is to destroy the formation of the cell wall membrane of the pathogen, causing the decomposition of the sporangia wall and causing the death of the pathogen. Except for the formation of zoospores and the swimming stage of the spores, it has effects on all stages of the oomycete, especially for the sporangia The formation stage of stalk and oospore is more sensitive. If the drug is used before the formation of sporangia and sporulation, the production of spores can be completely inhibited. Dimethomorph is especially effective against downy mildew and Phytophthora fungus, and can be used for grapes, potatoes and tomatoes, etc. Crop has the characteristics of less dosage, long duration and safe use, and has a good market prospect; in the existing dimethomorph production method, single sodium tert-butoxide or sodium amide is used as 3,4-dimethoxy- 4-Chloro-benzophenone and acetylmorpholine are basic catalysts for synthesizing dimethomorph. The catalytic effect is general. The chemical properties of sodium tert-butoxide and sodium amide are unstable and decompose when they meet water, resulting in a gradual decrease in catalytic effect and making the product Dimethomorph conversion and reduced purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]1) Synthesis of 芦 ether

[0021]1250 kg of distilled water was added to the reactor under nitrogen protection, and then 750 kg of phypsol was added to the reactor, and the 1866 kg of sodium hydroxide solution was added dropwise at 15 ° C, and the total time was controlled at 50 min, and after the drop was completed at 10 At ° C for 30 min, 2025 kg of dimethyl sulfate was added dropwise to the reactor under 20 ° C, and the total drip addition time was 2.7 h, then add 117 kg of sodium hydroxide solution. After 8 minutes, 117 kg sodium hydroxide was added again. The solution was heated to 50 ° C for 1 h, and 117 kg of dimethyl sulfate was added, and the mixture was allowed to stand for 10 min to the layered, then the reaction kettle water layer material and the emulsified layer material were transferred to the washed kettle, and the oil layer material rested to the reaction. Within the kettle, 600 ml of toluene was added to the reactor, warmed to 60 ° C, stirred for 30 min to stand ...

Embodiment 2

[0029]1) Synthesis of 芦 ether

[0030]1250 kg of distilled water was added to the reactor under nitrogen protection, and then 750 kg of phypsol was added to the reactor, and the 1866 kg of sodium hydroxide solution was added dropwise under 23 ° C, and the total time was controlled at 60 min, and after the drop was completed after 12 At ° C stirred at ° C, 2025 kg of dimethyl sulphate was added to the reactor under 25 ° C, and the total droplet addition time was 3.0 h, then the sodium hydroxide solution was 117 kg, and after 10min, 117 kg of sodium hydroxide was added again. The solution was warmed to 50 ° C for 1 h, and 117 kg of dimethyl sulfate was added, and the mixture was allowed to stand for 60 min to the layered, and then the reaction kettle was transferred to the water layer material and the emulsified layer. The oil layer material rested to the reaction. Within the kettle, 600 ml of toluene was added to the reaction kettle, warmed to 63 ° C, stirred for 35min to stand for 60 m...

Embodiment 3

[0038]1) Synthesis of 芦 ether

[0039]1250 kg of distilled water was added to the reactor under nitrogen protection, and then 750 kg of phthal phenol was added to the reaction kettle, and the 1866 kg of sodium hydroxide solution was added dropwise at 30 ° C, and the total time was controlled at 70 min, and after the drop was finished after 15. At ° C at ° C for 60 min, 2025 kg of dimethyl sulphate was added to the reactor under 30 ° C, and the total droplet time was 3.2 h, then the sodium hydroxide solution was added to 117kg, and after 12min, 117 kg sodium hydroxide was added again. The solution was warmed to 50 ° C for 1 h, and 117 kg of dimethyl sulfate was added, and the mixture was allowed to stand for 70min to the layered, then the reaction kettle material and the emulsified layer were transferred to the washed kettle, the oil layer material rested to the reaction. Within the kettle, 600 ml of toluene was added to the reaction kettle, warmed to 65 ° C, stirred for 40min to stand ...

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PUM

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Abstract

The invention discloses a production method of dimethomorph in the technical field of pesticide production. The production method comprises the following steps: 1) synthesis of veratrole, 2) 3,4-dimethoxy-4-chloro-diphenyl Ketone synthesis, 3) acetylmorpholine synthesis and 4) dimethomorph synthesis; synthesis of dimethomorph using sodium tert-butoxide as 3,4‑dimethoxy‑4‑chloro‑benzophenone and acetylmorpholine Basic catalyst, increase the step of using sodium hydroxide solution to carry out alkaline washing of the reactants in the reactor, and sodium hydroxide synthesizes dimethoxy morpholine from 3,4-dimethoxy-4-chloro-benzophenone and acetylmorpholine The morphine also has a catalytic effect, which makes up for the insufficiency of the gradual decrease in the catalytic effect of sodium tert-butoxide due to its unstable chemical properties when it encounters water and decomposes, and improves the conversion rate and purity of the product dimethomorph.

Description

Technical field[0001]The present invention relates to the field of pesticide production, and the specific area is a method for producing an alkenyl morpholine.Background technique[0002]Pesticide generalization refers to prevent, destroy or control diseases, insects, grass and other hazardous creatures that endanger agriculture and forestry through a purposeful regulation, control and development of hazardous organisms, growth, development and reproduction, and controlling agriculture and forestry; in daily life The narrow understanding is that it is guaranteed in agricultural production, promoting the growth of plants and crops, and a class of drugs administered, sterilized or harmful weeds are collectively referred to, and-alkenyl morpholine is an endotramal aimal low toxic sterilization The mechanism of action is to destroy the formation of the pathogenic wall film, causing the decomposition of the spore capsule to death, except for the formation of swivel spores and spores, each ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/185
CPCC07D295/185
Inventor 李华苏复刘利平
Owner 江苏恒隆作物保护有限公司
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