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Novel synthesis method of propyzamide

A technology of propargyl and a synthesis method, which is applied in the new synthesis field of propargyl, can solve the problems of poor product quality and long reaction time, and achieves the advantages of short reaction time, good product quality and shortened reaction time. Effect

Active Publication Date: 2021-04-16
HANDAN RUITIAN PESTICIDES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a novel synthesis method of benzamid, which solves the problems of long reaction time and poor product quality in the related art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 209.50 g of 3,5-dichlorobenzoyl chloride, 83.16 g of 3-amino-3-methyl-1-butyne, and 419.5 g of DMF (N,N-dimethylformamide) into the reactor, and start stirring , the temperature was raised to 20°C, 21.1g of potassium carbonate, 1.57g of cyclodextrin, and 4.72g of octyldodecyl xyloside were added to the reaction kettle, and the reaction was carried out for 5 hours. After the reaction was completed, 82.17g of water was added to the reaction solution, and two Chloroethane 246.52g, standing for stratification, adding sulfuric acid solution with a concentration of 2.0mol / L to 3.0mol / L to the stratified organic phase, adjusting the pH to 6-7, cooling to -5°C and stirring for 2 hours, After centrifugal filtration, 250.96 g of benzamide product was obtained, with a yield of 97.98% and a purity of 99.15%.

Embodiment 2

[0023] Put 209.48g of 3,5-dichlorobenzoyl chloride, 91.44g of 3-amino-3-methyl-1-butyne, and 523.75g of DMF (N,N-dimethylformamide) into the reactor, and start stirring , warming up to 20°C, adding 21.44g of potassium carbonate, 2.11g of cyclodextrin, and 6.29g of octyldodecyl xyloside to the reaction kettle, and reacted for 5 hours. After the reaction was completed, 94.86g of water was added to the reaction liquid, and two Chloroethane 284.53g, standing for stratification, adding sulfuric acid solution with concentration of 2.0mol / L~3.0mol / L to the organic phase after stratification, adjusting pH to 6~7, cooling to -5°C and stirring for 2 hours, After centrifugal filtration, 249.91 g of benzamid product was obtained, with a yield of 97.57% and a purity of 99.13%.

Embodiment 3

[0025] Put 209.51g of 3,5-dichlorobenzoyl chloride, 99.76g of 3-amino-3-methyl-1-butyne, and 838.75g of DMF (N,N-dimethylformamide) into the reactor, and start stirring , the temperature was raised to 20°C, 41.91g of potassium carbonate, 2.09g of cyclodextrin, and 8.38g of octyldodecyl xyloside were added to the reaction kettle, and the reaction was performed for 4 hours. After the reaction was completed, 133.35g of water was added to the reaction liquid, and two Chloroethane 400.14g, layered, add the layered organic phase to a sulfuric acid solution with a concentration of 2.0mol / L~3.0mol / L, adjust the pH to 6~7, cool down to -5°C and stir for 2 hours, then centrifugally filter 249.01 g of the benzamid product was obtained, with a yield of 97.22% and a purity of 99.11%.

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Abstract

The invention relates to the technical field of pesticide synthesis, and provides a novel synthesis method of propyzamide, which comprises the following steps: S1, adding 3, 5-dichlorobenzoyl chloride, 3-amino-3-methyl-1-butyne and a solvent into a reaction kettle, and starting stirring; S2, heating to 20 DEG C, adding an acid-binding agent and a compound catalyst into the reaction kettle, and reacting for 4-6 hours; S3, after the reaction is finished, adding water, adding dichloroethane, and layering; S4, adding the layered organic phase into a sulfuric acid solution with the concentration of 2.0 mol / L-3. 0mol / L, regulating the pH value to 6-7, cooling to 5 DEG C, stirring for 2 hours, and centrifugally filtering to obtain the propyzamide product. Through the technical scheme, the problems of long reaction time and poor product quality in the prior art are solved.

Description

technical field [0001] The invention relates to the technical field of pesticide synthesis, in particular to a novel synthesis method of benzamid. Background technique [0002] Propyramide, N-(1,1-dimethylpropargyl)-3,5-dichlorobenzamide, also known as Nazat, is a benzamide herbicide, CAS23950- 58-5. It is a selective post-emergence herbicide. Penpyramide is a herbicide for weeds and certain perennial weeds in small-seeded leguminous crops, peanuts, soybeans, potatoes, lettuce, and certain orchard cash crops. [0003] The preparation method disclosed in CN 107903181 B is that 3,5-dichlorobenzoyl chloride is added dropwise to a mixed solution of 3-amino-3-methyl-1-butyne, sodium hydroxide, triethylamine and dichloromethane . The disadvantages of this process are poor reaction time, poor product color, low yield and low content. Contents of the invention [0004] The invention proposes a novel synthesis method of benzamid, which solves the problems of long reaction time...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/65
Inventor 王鹏飞王学铭马立香张艳敏
Owner HANDAN RUITIAN PESTICIDES CO LTD
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