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The production method of propargyl flufenamide

A technology of flufenazim propargyl and its production method, which is applied in the direction of organic chemistry, can solve problems such as the difficulty in preparing high-content products, no post-processing methods, and complicated nitro group positioning, so as to solve the problems of large-scale production and production The effect of low cost and high product purity

Active Publication Date: 2018-04-24
SICHUAN YIJIE TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The price of the selected raw material m-difluorobenzene is relatively low, but the positioning of the nitro group is complicated when it is nitrated, there are many by-products, and the separation is difficult. Relatively speaking, it is difficult to prepare high-content products
[0008] In summary, there is still no process route that is easy for large-scale production, and there are basically no reports about the post-treatment method of industrial production. For this reason, the patent of the present invention has developed a process for the large-scale production of flufenazine propargyl , to solve the predicament of domestic imitation production of diflufenamide and improve market competitiveness

Method used

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  • The production method of propargyl flufenamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] a pressfigure 1 The production method of the propargyl flurafen that shown reaction formula carries out, it may further comprise the steps:

[0045] (1) Nitrification reaction

[0046] Inject 42.5kg of fuming nitric acid and 280kg of 98% concentrated sulfuric acid into the reaction kettle, control the temperature at 20-30°C, then add 100kg of 2,4-difluoronitrobenzene dropwise under stirring conditions, and control the reaction temperature during the dropwise addition The temperature is 20-45°C. After the dropwise addition, the temperature is raised to 50°C and reacted for at least 1 hour. Then take 0.5mL of stirring liquid, add 0.5mL of dichloroethane, take the upper organic phase, wash it with water, and then detect it under the condition of liquid phase analysis. The mass content of 2,4-difluoronitrobenzene, when the mass content of 2,4-difluoronitrobenzene is less than 0.2%, add 200kg 1,2-dichloroethane to the reaction kettle for extraction and layering, The obtaine...

Embodiment 2

[0059] The difference between this example and Example 1 is that in step (2) etherification reaction, when the mass content of 1,5-difluoro-2,4-dinitrobenzene is less than 6%, the reaction system Add soft water to quench the phase separation, and the lower layer solution after phase separation uses NaHCO 3 Solution is carried out alkali washing, and other steps are identical with embodiment 1.

Embodiment 3

[0061] The present embodiment differs from Examples 1 to 2 in that: step (2) the lower layer solution after the etherification reaction is quenched and phase-separated uses Na 2 CO 3 Solution is carried out alkali washing, and other steps are identical with embodiment 1 or 2.

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Abstract

The invention discloses a production method of flumioxazin. The production method comprises the following steps: by using 2,4-difluoronitrobenzene as an initial raw material, sequentially carrying out nitrification to obtain 1,5-difluoro-2,4-dinitrobenzene, and carrying out etherification reaction on the 1,5-difluoro-2,4-dinitrobenzene and butyl hydroxyacetate to obtain butyl 3-fluoro-4,6-dinitrophenoxyacetate; carrying out reduction cyclization with hydrogen to obtain 7-fluoro-6-amino-2H-1,4-benzoxazinyl-3(4H)-one; under alkaline conditions, carrying out alkynylation reaction with propargyl chloride to obtain an intermediate product; and finally, carrying out amidation reaction with 3,4,5,6-tetrahydrophthalic anhydride to obtain the flumioxazin. The production technique of the method has the advantages of short process, mild reaction conditions and cheap and accessible raw materials, and is convenient to operate; and the solvent used in the preparation process is recyclable. The method also has the advantages of high total reaction yield, high product purity, low production cost and low environmental pollution.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a production method of fluflumecil propargyl. Background technique [0002] Flurafen propargyl is a phthalimide herbicide developed by Sumitomo Industrial Chemicals Co., Ltd., Japan. It is also a typical contact herbicide, but it cannot be used for post-emergence stem and leaf treatment. After the soil surface is treated with flufenamide propargyl, the agent is absorbed by the soil particles and a treatment layer is formed on the soil surface. When the weeds germinate, the seedlings will die when they contact the agent treatment layer; when the stems and leaves are treated, the plant sprouts and leaves Absorption, conduction in the body, rapid action on the leaves of sensitive weeds, causing the accumulation of protoporphyrin, enhancing the peroxidation of cell membranes, resulting in irreversible damage to the cell membrane structure and cell functions of sensitive weeds. After spraying...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D413/04
CPCC07D413/04
Inventor 吴志兵唐猷成覃攀
Owner SICHUAN YIJIE TECH CO LTD
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