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A kind of synthetic method of emamectin benzoate

A technology of methylamino abamectin and benzoate, which is applied in the field of organic synthesis, can solve the problems of many by-products, complicated preparation process and high cost, and achieves the reduction of operating staff, cost reduction, and stable process and quality. Effect

Active Publication Date: 2021-01-01
HUBEI JINGHONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of this invention is to solve the complex preparation process of existing emamectin benzoate, the cost is higher, and the problem that by-products are more, and a kind of synthetic emamectin benzoate is provided formate method

Method used

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  • A kind of synthetic method of emamectin benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First step single protection

[0035] Put 100KG of abamectin, 300KG of dioxane and 0.4KG of concentrated hydrochloric acid into the kettle, cool down to -20°C, add 9KG of vinyl ether dropwise, control the temperature below -18°C, raise the temperature to room temperature and stir after the addition is completed Overnight, the detection reaction was complete. If there are any remaining raw materials, add 2-5% vinyl ether appropriately, and continue stirring until the reaction is complete.

[0036] second oxidation

[0037] Add 18KG of dimethyl sulfoxide and 15KG of tetramethylethylenediamine to the above solution, cool down to -15°C, add 24KG of phenyl phosphate dichloride dropwise, and react for 5-8 hours after the dropwise addition, and detect that the reaction is complete. Filter through celite, to be used in the next reaction.

[0038] The third step imidization

[0039] Add the solution obtained in the second step into the kettle, 28KG of methylamino alcohol sol...

Embodiment 2

[0045] First step single protection

[0046] Put 100KG of abamectin, 300KG of diethoxymethane and 0.4KG of concentrated hydrochloric acid into the kettle, cool down to -20°C, add 9KG of vinyl ether dropwise, control the temperature below -18°C, and rise to room temperature after the addition is completed Stir overnight and check for complete reaction.

[0047] second oxidation

[0048] Add 18KG of dimethyl sulfoxide and 15KG of tetramethylethylenediamine to the above solution, cool down to -15°C, add 24KG of phenyl phosphate dichloride dropwise, and react for 4-5 hours after the dropwise addition, and detect that the reaction is complete. Filter through celite, to be used in the next reaction.

[0049] The third step imidization

[0050] Add the solution obtained in the second step into the kettle, 28KG of methylamino alcohol solution. After mixing evenly, control the temperature in the kettle at 0° C., react for 3 hours, and check that the reaction is complete. If the rea...

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Abstract

The invention discloses a synthetic method of emamectin benzoate, which belongs to the technical field of organic synthesis. According to the method, avermectin is taken as a raw material, through single protection-oxidation-imidization-reduction-deprotection salt-forming, the emamectin benzoate is obtained. The scheme has the advantages that the cost is low, the period is short, the yield of theprepared emamectin benzoate is more than 85%, and the fine product content can reach 98%. Through production validation, the technology and quality are stable, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of emamectin benzoate, which belongs to the technical field of organic synthesis. Background technique [0002] Emamectin benzoate, full name emamectin benzoate, white or light yellow crystalline powder, soluble in acetone and methanol, slightly soluble in water, insoluble in hexane. Compared with avermectin, the insecticidal activity has been improved by 3 orders of magnitude at first, and it has a very high activity on the larvae of Lepidoptera insects and many other pests. It has both gastric toxicity and contact action. 2g / ha) has a very good effect, and does not harm beneficial insects in the process of controlling pests, which is conducive to the comprehensive control of pests, and in addition, it expands the insecticidal spectrum and reduces the toxicity to humans and animals. [0003] The synthetic method of emamectin emamectin follows the production process reported by Raymond J.Cvetovich in 1994, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/00
CPCC07H1/00C07H17/08
Inventor 杨辉崔军霞莫思霜王勇丽
Owner HUBEI JINGHONG CHEM
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