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5-dichloroacetyl-3,6-dimethyl-3-ethyl-9-oxa-1,5-diazabicyclo[4.3.0]nonane and synthetic method

A technology of dichloroacetyl and diazabicyclo is applied in the directions of botanical equipment and methods, animal repellents, biocides, etc., and can solve the problems of high reaction temperature, long reaction time, complicated operation, etc. The effect of mild conditions, short response time and high promotion value

Inactive Publication Date: 2009-03-11
NORTHEAST AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are disadvantages such as high cost of raw materials, long reaction time, complicated operation, high reaction temperature, many by-products, and serious environmental pollution in the technology of synthesizing the above-mentioned various compounds.
At present, there is no report about the azadichloroacetamide herbicide safener and its synthesis method. About the compound 5-dichloroacetyl-3,6-dimethyl-3-ethyl-9-oxa -1,5-diazabicyclo[4.3.0]nonane has not been reported on the synthesis method and biological activity

Method used

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  • 5-dichloroacetyl-3,6-dimethyl-3-ethyl-9-oxa-1,5-diazabicyclo[4.3.0]nonane and synthetic method
  • 5-dichloroacetyl-3,6-dimethyl-3-ethyl-9-oxa-1,5-diazabicyclo[4.3.0]nonane and synthetic method
  • 5-dichloroacetyl-3,6-dimethyl-3-ethyl-9-oxa-1,5-diazabicyclo[4.3.0]nonane and synthetic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0017] Example: Synthesis of 2-methyl-2-ethyl-1,3-dinitropropane

[0018] Add 27mL of butanone, 48mL of nitromethane, and 6mL of hexahydropyridine into a three-neck flask, stir evenly, heat at 90-94°C, reflux for 18 hours, cool to room temperature, and adjust the pH of the solution to weak acidity with 2mol / L hydrochloric acid , separate the oil layer, extract the water layer with chloroform, dry the organic layer with anhydrous sodium sulfate, and distill under reduced pressure to collect the fraction at 135~138°C / 9mmHg. The product is a light yellow oily liquid with a pungent smell, and the yield is 54.7%. . The equation is as follows:

[0019]

[0020] Synthesis of 2-methyl-2-ethyl-1,3-propanediamine

[0021] In a 500mL three-necked flask equipped with a dropping funnel, an electric stirrer and a reflux condenser, add 50g of reduced iron powder, 70mL of water, and 2.0mL of concentrated hydrochloric acid in sequence, heat, stir with an electric stirrer and boil slightly...

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Abstract

The invention relates to 5-dichloroacetyl-3, 6-dimethyl-3-ethyl-9-oxa-1, 5-diazabicylo (4.3.0) nonane and a synthesis method thereof, which belong to the organic synthesis technology. The structural formula of the 5-dichloroacetyl-3, 6-dimethyl-3-ethyl-9-oxa-1, 5-diazabicylo (4.3.0) nonane is as shown in a figure. The synthesis method is as follows: firstly, an acetylpropionic acid and 2-methyl-2-ethyl-1, 3-propylene diamine are taken as raw materials, and water in a system is separated in a solvent by the reflux water diversion method; secondly, the temperature of the system is reduced to 50 DEG C, and an acid-binding agent is added into the system to make the pH value of the system maintain 8.4; thirdly, the temperature of the system is controlled, dichloroacetyl chloride is dripped into the system to maintain constant pH value, and is stirred for a certain period; and fourthly, organic phases are washed into neutrality, and the product of the 5-dichloroacetyl-3, 6-dimethyl-3-ethyl-9-oxa-1, 5-diazabicylo (4.3.0) nonane is obtained after drying through anhydrous MgSO4, removal of a solvent and recrystallization of obtained coarse products by ethyl acetate-petroleum ether. The product and the method have the advantages of easily obtained raw materials, high yield, simple operation, short reaction period, low production cost and no environmental pollution.

Description

technical field [0001] The invention belongs to the technical fields of organic synthesis and pesticide synthesis, and in particular relates to a herbicide safener and a synthesis method thereof. Background technique [0002] Herbicide safeners selectively protect crops from herbicide damage without affecting the activity of herbicides on target weeds. Since herbicide safeners have multiple functions and effects, they have developed rapidly in the past ten years, and have developed into various types to detoxify different types of herbicides. At present, herbicide safeners at home and abroad mainly include: naphthalene pyrones, dichloroacetamides, dichloromethanedioxolanes, oxime ether derivatives, substituted thiazole derivatives, phenylpyrimidines, triazole carboxyl Acids and quinoline and acetates, etc. In recent years, the dichloroacetamide herbicide safeners developed in succession include: AD-67, R-29148, MON13900, dichloroacrylamine, oxazone, etc. However, there ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04A01N25/32A01P13/00
Inventor 叶非付颖赵李霞孙太凡
Owner NORTHEAST AGRICULTURAL UNIVERSITY
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