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Synthesis method of clodinafop-propargyl

A synthetic method, the technology of clodinafop-propargyl, which is applied in the field of synthesis of clodinafop-propargyl, can solve the problems of affecting the quality of clodinafop-propargyl products, low synthesis efficiency, cumbersome synthesis steps, etc.

Inactive Publication Date: 2021-01-22
甘肃联凯生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The content of 2,3-difluoro-5-chloropyridine currently available on the market is basically about 96%, of which 3% (area normalization method) isomers, in the synthesis process of clodinafop-propargyl Among them, the above-mentioned 3% (area normalization method) isomers will eventually form about 3% (area normalization method) isomers of clodinafop-propargyl as the reaction proceeds, which will affect the final clodinafop-propargyl product quality
[0003] In order to improve the purity of the clodinafop-propargyl product, there are generally purification steps in the currently disclosed synthetic route of clodinafop-propargyl, which makes the synthesis steps more cumbersome and the synthesis efficiency is low

Method used

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  • Synthesis method of clodinafop-propargyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0018] Dissolve 72.9g (0.4mol) DHPPA in 200g acetonitrile, stir and heat up, add 0.3g sodium sulfite and 55g (0.97mol) KOH at 50°C, and start adding 66g of 2,3-difluoro-5-chloropyridine dropwise when the temperature rises to 60°C (0.44mol), after the dropwise addition, the temperature was raised to 70°C for 5 hours. After the heat preservation, remove acetonitrile under reduced pressure, add 200g of water after removing acetonitrile, add dropwise hydrochloric acid with a mass fraction of 30% to adjust pH = 1, cool and precipitate, filter, and wash with water to obtain a dry etherified product: 124.6g.

[0019] Feed 62.3g (about 0.2mol) of ether compound and 82g of DMF into a 500mL four-necked bottle and heat up until the material is completely dissolved. Add 30g (0.22mol) of potassium carbonate and heat up to 60°C. Add 20g (0.27mol) of propyne chloride dropwise. Finish at 65°C for 4 hours. Heat preservation finishes adding water 100g, toluene 130g, stirring and dissolving, st...

Embodiment approach 2

[0021] Dissolve 72.9g (0.4mol) of DHPPA in 200g of acetonitrile, stir and heat up, add 0.3g of sodium sulfite and 53.3g (0.95mol) of KOH at 50°C, and start adding 2,3-difluoro-5-chloropyridine dropwise when the temperature rises to 60°C 66g (0.44mol), the dropwise addition was completed and the temperature was raised to 70°C for 5 hours. After the heat preservation is over, remove acetonitrile under reduced pressure, add 200 g of water after removing the acetonitrile, add dropwise hydrochloric acid with a mass fraction of 30% to adjust pH = 1, cool and precipitate, filter, and wash with water to obtain a dry etherified product: 124 g.

[0022] Feed 62g (about 0.2mol) of ether compound and 82g of DMF into a 500mL four-necked bottle and heat up until the material is completely dissolved. Add 30g (0.2mol) of potassium carbonate and heat up to 60°C. Add 20g (0.27mol) of propyne chloride dropwise, and the addition is completed Incubate at 65°C for 4 hours. Heat preservation finish...

Embodiment approach 3

[0024] Dissolve 72.9g (0.4mol) of DHPPA in 200g of acetonitrile, stir and raise the temperature, add 0.3g of sodium sulfite and 56.1g (1mol) of KOH at 50°C, and start adding 2,3-difluoro-5-chloropyridine 74.7 dropwise at 60°C g (0.5mol), after the dropwise addition, the temperature was raised to 70°C for 6 hours. After the heat preservation is over, remove acetonitrile under reduced pressure, add 200 g of water after removing the acetonitrile, add dropwise hydrochloric acid with a mass fraction of 30% to adjust the pH to 1, cool and precipitate, filter, and wash with water to obtain a dry etherified product: 130 g.

[0025] Feed 65g (about 0.2mol) of ether compound and 82g of DMF into a 500mL four-necked bottle and heat up until the material is completely dissolved. Add 30g (0.22mol) of potassium carbonate and heat up to 60°C. Add 20g (0.27mol) of propyne chloride dropwise, and the addition is completed Incubate at 65°C for 4 hours. Heat preservation finishes adding water 100...

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Abstract

The invention relates to the field of chemical engineering, and discloses a synthesis method of clodinafop-propargyl. The method comprises the following steps of: dissolving DHPPA in an organic solvent, heating to a temperature of 50 DEG C, adding an antioxidant and potassium hydroxide, heating to a temperature of 60 DEG C, starting to dropwise add 2, 3-difluoro-5-chloropyridine, heating to a temperature of 70 DEG C after completing the dropwise addition; removing the organic solvent under reduced pressure after heat preservation is finished, adding water after the organic solvent is completely removed, adjusting the pH value to be 1-2, cooling and separation are carried out, performing filtering, performing washing with water to obtain etherate; dissolving the etherate in DMF, heating until the etherate is completely dissolved, adding potassium carbonate, heating to 60 DEG C, dropwise adding propargyl chloride, and keeping the temperature at 60-70 DEG C after after completing the dropwise addition; after completing heat preservation, adding water and methylbenzene, stirring for dissolving, performing still standing for layering, and washing; and decolorizing an organic layer, performing filtering, desolventizing a filtrate with water vapor, and performing slicing to obtain the clodinafop-propargyl finished product. According to the synthesis method, on the premise that a purification step is omitted, the isomeride in the clodinafop-propargyl product is controlled to be about 1% (area content).

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for synthesizing clodinafop-propargyl. Background technique [0002] The content of 2,3-difluoro-5-chloropyridine currently available on the market is basically about 96%, of which 3% (area normalization method) isomers, in the synthesis process of clodinafop-propargyl Among them, the above-mentioned 3% (area normalization method) isomers will eventually form about 3% (area normalization method) isomers of clodinafop-propargyl as the reaction proceeds, which will affect the final clodinafop-propargyl product quality. [0003] In order to improve the purity of the clodinafop-propargyl product, the currently disclosed synthetic route of clodinafop-propargyl generally has a purification step, which makes the synthetic steps more cumbersome and the synthesis efficiency is low. Contents of the invention [0004] Purpose of the invention: Aiming at the problems existing in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/643
CPCC07D213/643
Inventor 赵飞四覃能东任永辉蒋云翔
Owner 甘肃联凯生物科技有限公司
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