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Preparation method of fomesafenbulk drug intermediate acifluorfen

A technology of fomesafen and acifluorfen is applied in the field of preparation of acifluorfen technical intermediate of fomesafen, and can solve the problems of high nitration reaction temperature, low content yield and high reaction temperature , to achieve the effect of reducing nitrification temperature, high safety and increasing content

Inactive Publication Date: 2020-09-01
山东滨海瀚生生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this synthetic route reaction temperature is higher, safety is lower, and content yield is on the low side, and its main reason is: under this reaction condition, nitration reaction temperature is high, side reaction is more, selectivity is poor, content is on the low side

Method used

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  • Preparation method of fomesafenbulk drug intermediate acifluorfen
  • Preparation method of fomesafenbulk drug intermediate acifluorfen
  • Preparation method of fomesafenbulk drug intermediate acifluorfen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 31.6g (actual dosage) of 3-[2-chloro-4-(trifluoromethyl)phenoxy]benzoic acid of 90.6% content and put it into a 500ml reaction bottle, add 170ml dichloroethane, stir and heat up Dissolve, cool down to about 55°C and add 30.6g of acetic anhydride, continue to cool down to 0°C, start to add 28.3g of mixed acid (0.16mol of concentrated nitric acid and 0.18mol of concentrated sulfuric acid) dropwise, the temperature does not exceed 5°C during the dropwise addition. After the dropwise addition was completed, the temperature was naturally raised to between 20°C and 25°C, and the temperature was maintained for 1.5 hours to carry out the reaction. After the reaction is completed, add 10ml of water dropwise at a controlled temperature of 50-55°C. After the dropwise addition is completed, stir at a controlled temperature of 55-60°C for 30 minutes, let stand for stratification, and remove the spent acid. After the waste acid is separated, add 100ml of water to control the te...

Embodiment 2

[0031] Weigh 31.6g (actual dosage) of 3-[2-chloro-4-(trifluoromethyl)phenoxy]benzoic acid of 90.6% content and put it into a 500ml reaction bottle, add 170ml dichloroethane, stir and heat up Dissolve, cool down to about 55°C and add 30.6g of acetic anhydride, continue to cool down to 5°C and start adding 28.3g of mixed acid (concentrated nitric acid 0.16mol and concentrated sulfuric acid 0.18mol) dropwise, the temperature during the dropping process does not exceed 10°C. After the dropwise addition was completed, the temperature was naturally raised to between 20°C and 25°C, and the temperature was maintained for 1.5 hours to carry out the reaction. After the reaction is completed, add 10ml of water dropwise at a controlled temperature of 50-55°C. After the dropwise addition is completed, stir at a controlled temperature of 55-60°C for 30 minutes, let stand for stratification, and remove the spent acid. After the waste acid is separated, add 100ml of water to control the tempe...

Embodiment 3

[0033] Weigh 31.6g (actual dosage) of 3-[2-chloro-4-(trifluoromethyl)phenoxy]benzoic acid of 90.6% content and put it into a 500ml reaction bottle, add 170ml dichloroethane, stir and heat up Dissolve, cool down to about 55°C and add 27.8g of acetic anhydride, continue to cool down to 0°C, start to add 28.3g of mixed acid (0.16mol of concentrated nitric acid and 0.18mol of concentrated sulfuric acid) dropwise, the temperature does not exceed 5°C during the dropwise addition. After the dropwise addition was completed, the temperature was naturally raised to between 20°C and 25°C, and the temperature was maintained for 1.5 hours to carry out the reaction. After the reaction is completed, add 10ml of water dropwise at a controlled temperature of 50-55°C. After the dropwise addition is completed, stir at a controlled temperature of 55-60°C for 30 minutes, let stand for stratification, and remove the spent acid. After the waste acid is separated, add 100ml of water to control the te...

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Abstract

The invention provides a preparation method of fomesafenbulk drug intermediate acifluorfen, and belongs to the technical field of pesticides. According to the method, a low-temperature nitrification mode is adopted,nitrylions can be slowly released, so that the reaction tends to be gentle, the selective competitiveness of a target product is enhanced, polynitrification and ectopic nitrification byproducts are inhibited, and the content of the intermediate acifluorfen is effectively increased. The method provided by the invention can be effectively applied to production and application of the fomesafen technical.

Description

technical field [0001] The invention belongs to the technical field of pesticides, and in particular relates to a preparation method of acifluorfen, an intermediate of fomesafen technical medicine. Background technique [0002] Fomesafen, also known as Huwei, has a chemical name of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-N-methylsulfonyl-2-nitrobenzamide, which belongs to fluorine-containing diphenyl Ether herbicide is an inhibitor of protoporphyrinogen oxidase, and is a high-efficiency, low-toxicity, broad-spectrum upland herbicide. [0003] Acifluorfen is an intermediate in the synthesis of fomesafen technical, and its quality directly affects the quality of fomesafen technical. Therefore, the production of high-content acifluorfen has become a research topic for domestic enterprises. At present, most domestic synthesis uses 3-[2-chloro-4-(trifluoromethyl)phenoxy]benzoic acid as the starting material, which is obtained through high-temperature nitration. However, the sy...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C201/16C07C205/59
CPCC07C201/08C07C201/16C07C205/59
Inventor 刘谦陈会存吴本林张瑞生庞楠郭磊
Owner 山东滨海瀚生生物科技有限公司
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