Dimethomorph production method

A production method, dimethomorph technology, applied in the field of dimethomorph production, can solve problems such as death, reduction of dimethomorph conversion rate and purity, unstable chemical properties, etc.

Active Publication Date: 2018-04-20
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

[0024] 1) Synthesis of veratrole

[0025] Add 1250kg of distilled water to the reactor under the protection of nitrogen, then put 750kg of catechol into the reactor, drip 1866kg of sodium hydroxide solution at 15°C, and control the total time of dripping at 50min. Stir at ℃ for 30min, add 2025kg of dimethyl sulfate dropwise to the reactor at 20℃, the total dropping time is 2.7h, then add 117kg of sodium hydroxide solution, after an interval of 8min, add 117kg of sodium hydroxide again Solution, heat up to 50°C for 1 hour, add 117kg of dimethyl sulfate, stir for 10 minutes and let it stand for 50 minutes to separate layers, then transfer the water layer materials and emulsified layer materials in the reaction kettle to the water washing kettle, and the oil layer materials remain until the reaction In the kettle, add 600ml of toluene into the reaction kettle, raise the temperature to 60°C, stir for 30 minutes, then let it stand for 50 minutes until the layers are separated, and ...

Embodiment 2

[0033] 1) Synthesis of veratrole

[0034]Add 1250kg of distilled water to the reactor under the protection of nitrogen, then put 750kg of catechol into the reactor, drip 1866kg of sodium hydroxide solution at 23°C, and control the total time of dripping at 60min. Stir at ℃ for 45min, add 2025kg of dimethyl sulfate dropwise to the reaction kettle at 25℃, the total dropping time is 3.0h, then add 117kg of sodium hydroxide solution, after an interval of 10min, add 117kg of sodium hydroxide again Solution, heat up to 50°C for 1 hour, add 117kg of dimethyl sulfate, stir for 11 minutes and let it stand for 60 minutes to separate layers. In the kettle, add 600ml of toluene into the reaction kettle, raise the temperature to 63°C, stir for 35 minutes, then let it stand for 60 minutes until the layers are separated, and distill the veratrole;

[0035] 2) Synthesis of 3,4-dimethoxy-4-chloro-benzophenone

[0036] Under the protection of nitrogen, put the veratrole produced in step 1), 6...

Embodiment 3

[0042] 1) Synthesis of veratrole

[0043] Add 1250kg of distilled water to the reactor under the protection of nitrogen, then put 750kg of catechol into the reactor, drip 1866kg of sodium hydroxide solution at 30°C, and control the total time of dripping at 70min. Stir at ℃ for 60min, add 2025kg of dimethyl sulfate dropwise to the reaction kettle at 30℃, the total dropping time is 3.2h, then add 117kg of sodium hydroxide solution, after an interval of 12min, add 117kg of sodium hydroxide again Solution, heat up to 50°C for 1 hour, add 117kg of dimethyl sulfate, stir for 12 minutes and let stand for 70 minutes to separate layers, then transfer the water layer materials and emulsified layer materials in the reaction kettle to the water washing kettle, and the oil layer materials remain until the reaction In the kettle, add 600ml of toluene into the reaction kettle, raise the temperature to 65°C, stir for 40 minutes, then let it stand for 70 minutes until the layers are separated...

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PUM

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Abstract

The invention discloses a dimethomorph production method in the technical field of pesticide production. The production method comprises: 1) synthesizing veratrole; 2) synthesizing 3,4-dimethoxy-4-chloro-benzophenone; 3) synthesizing acetylmorpholine; and 4) synthesizing dimethomorph. Sodium tert-butoxide is taken as a basic catalyst for synthesizing dimethomorph from 3,4-dimethoxy-4-chloro-benzophenone and acetylmorpholine, and a sodium hydroxide solution is used to perform alkali washing on a reactant in a reaction vessel. Sodium hydroxide has a catalytic effect on synthesis of dimethomorphfrom 3,4-dimethoxy-4-chloro-benzophenone and acetylmorpholine. The defect that the catalytic effect of sodium tert-butoxide is gradually reduced due to unstable chemical property of sodium tert-butoxide and degradation of sodium tert-butoxide when sodium tert-butoxide comes into water is overcome. The dimethomorph product is improved in conversion rate and purity.

Description

technical field [0001] The invention relates to the technical field of pesticide production, in particular to a production method of dimethomorph. Background technique [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...

Claims

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Application Information

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Patent Type & Authority Applications(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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