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Improved method for synthesizing 1-acetyl-1-chlorocyclopropane

A synthesis method, the technology of chlorocyclopropane, which is applied in the field of synthesis of pesticide intermediates, can solve the problems of difficult processing, a large amount of tar, and high prices, and achieve the effects of avoiding environmental pollution, easy operation, and lower production prices

Inactive Publication Date: 2018-05-29
NUTRICHEM LAB CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But adopt this method, on the one hand be to use the phase-transfer catalyst with higher price, on the other hand because product is not stable under alkaline condition, reaction system still keeps alkaline after reaction is finished, need to classify product quickly, otherwise it will be A large amount of tar is produced, which brings difficulties to the treatment of subsequent processes

Method used

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  • Improved method for synthesizing 1-acetyl-1-chlorocyclopropane
  • Improved method for synthesizing 1-acetyl-1-chlorocyclopropane
  • Improved method for synthesizing 1-acetyl-1-chlorocyclopropane

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add sodium carbonate (0.15mol) and 100g acetonitrile to a 250ml four-neck bottle, start stirring, and add 3,5-dichloro-2-pentanone ( 0.1mol), 10min after dripping, heat preservation reaction for 5-6h, gas phase control detection 3,5-dichloro-2-pentanone < 1%, the reaction is considered complete, the system is cooled to 25 ° C, suction filtration, filtrate rectification Acetonitrile was recovered, and the still residue was continued to rectify to obtain the product (weight 9.8g). The reaction yield was 85.0%, and the isolated yield was 83.0%.

Embodiment 2

[0027] Add sodium bicarbonate (0.3mol) and 100g acetonitrile to a 250ml four-necked bottle, start stirring, heat the system to 80-85°C, add 3,5-dichloro-2-pentanone dropwise at this temperature (80-85°C) (0.1mol), after 10 minutes of dripping, heat preservation reaction for 10 hours, gas phase control, detection of 3,5-dichloro-2-pentanone <1%, as the reaction is complete, the system is cooled to 25 ° C, suction filtration, filtrate rectification Collect the solvent and continue to rectify to obtain the product with a weight of 9.30 g, a reaction yield of 83.1%, and an isolation yield of 80.4%.

Embodiment 3

[0029] In a 250ml four-necked bottle, add sodium carbonate (0.15mol), 100g of N-methylpyrrolidone, start stirring, heat the system at 100-110°C, add 3,5-dichloro-2 -Pentanone (0.1mol), after 10 minutes of dripping, keep warm for 2 hours, control in the gas phase, detect 3,5-dichloro-2-pentanone < 1%, the reaction is considered complete, cool the system to 25°C, filter with suction, The filtrate is rectified to collect solvent and product. The weight is 9.4 g, the reaction yield is 82.8%, and the isolated yield is 79.3%.

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Abstract

The invention discloses an improved method for synthesizing 1-acetyl-1-chlorocyclopropane. The method uses 3,5-dichloro-2,2-pentanone as a raw material for heating for reaction in an inorganic base and an organic solvent. By use of optimized reaction conditions, a product is synthesized and purified by distillation. By adopting the method, the production price of the product is reduced, generationof a waste solvent is reduced, and environment is not polluted. In addition, the distillation process is simple in operation and easy to operate, can be widely used in industrial production, and is conducive to the industrialization of the product.

Description

Technical field: [0001] The invention relates to the field of chemical pesticide production, in particular to a method for synthesizing a pesticide intermediate. technical background: [0002] Prothioconazole is a new type of broad-spectrum triazolethione fungicide, which is mainly used to prevent and control many diseases on wheat, barley, rape, peanut, rice and beans, and has great effect on almost all wheat diseases. Good control effect. The fungicide has many advantages such as broad spectrum, low toxicity, good systemic absorption, long-lasting effect, various spraying methods, and no environmental risk concerns. It is recognized as one of the most promising triazole fungicides. [0003] As an important intermediate in the synthesis process of prothioconazole, the synthesis of 1-acetyl-1-chlorocyclopropane has attracted more and more attention from researchers. At present, the common method for synthesizing 1-acetyl-1-chlorocyclopropane is The 3,5-dichloro-2-pentanone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/67C07C49/327
CPCC07C45/67C07C49/327
Inventor 焦体孙自培李辛夷汪春华
Owner NUTRICHEM LAB CO LTD
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