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Synthesis method of flumioxazin

A technology of profenachlor and a synthesis method, which is applied in the field of pesticide synthesis, can solve the problems of high price, high toxicity, and large environmental pollution caused by iron powder reduction, and achieves the effects of simple operation, few by-products, and low environmental protection pressure.

Inactive Publication Date: 2020-01-07
SHANGYU JINTENG MEDICAL CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In this synthetic route, iron powder reduction ring-closing pollution is relatively large, and 3-bromopropyne is expensive and toxic as a propynylation reagent

Method used

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  • Synthesis method of flumioxazin
  • Synthesis method of flumioxazin
  • Synthesis method of flumioxazin

Examples

Experimental program
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Effect test

Embodiment 1

[0046] 1. Synthesis of 1,5-difluoro-2,4-dinitrobenzene (BQ-2)

[0047] First, m-dichlorobenzene is used as a raw material, 70% nitric acid is used as a nitrating reagent, and dichloroethane (DCE) is used as a solvent to react to obtain 1,3-dichloro-4,6-dinitrobenzene; 1,3-dichlorobenzene Chloro-4,6-dinitrobenzene was fluorinated to obtain 1,5-difluoro-2,4-dinitrobenzene (BQ-2);

[0048] 2. Synthesis of isopropyl 3-fluoro-4,6-dinitrophenoxyacetate (BQ-3)

[0049]Put into the flask BQ-2, DMF (dimethylformamide), isopropyl chloroacetate, potassium hydroxide, stir to be warmed up to 120 ° C, and keep the reaction for 3 hours, after the intermediate control conversion is qualified (the conversion rate reaches more than 98%) ), cooled to room temperature, the salt residue was removed by suction filtration, the salt residue was rinsed with a small amount of fresh DMF, the filtrate was distilled under reduced pressure, the vacuum degree of the distillation process was -0.09MPa, and t...

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Abstract

The invention provides a synthesis method of flumioxazin, and belongs to the field of pesticide synthesis. According to the invention, the method solves the problems of many steps, low yield and the like in the existing flumioxazin synthesis process, has the following synthetic route defined in the specification, and has high yield.

Description

technical field [0001] The invention belongs to the field of pesticide synthesis, in particular to a method for synthesizing flumechlor propargyl. Background technique [0002] Propyramide is an N-phenylphthalimide herbicide listed by Japan's Sumitomo Chemical Industry Co., Ltd. in 1993. It is mainly used for the control of grass weeds and broadleaf on soybeans, sugarcane, cotton and other crops. leaf weeds. The synthetic method of propargyl flufenamide currently has the following types: [0003] (1) Using m-fluorophenol as raw material, it is prepared through 5-step reactions including fluorine hydrolysis, nitration, cyclization, propynylation, and phthalic anhydride acylation. [0004] [0005] The raw material m-fluorophenol used in this synthesis route is expensive; after hydrolysis, ether bonds are generated and then nitrated, but due to the severe nitration reaction conditions, it is easy to cause the breakage of ether bonds; using iron powder for hydrogenation re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/04
CPCC07D413/04
Inventor 易克炎尹凯徐伟伟杜明于江柴华强徐新
Owner SHANGYU JINTENG MEDICAL CHEM IND