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Synthesis process of acaricide of emamectin benzoate

A synthetic process, the technology of emamectin benzoate, which is applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., can solve the problems of difficulty in developing new pesticides and low success rate of product development, and achieve huge market potential and increase Purity, promising effect

Inactive Publication Date: 2017-01-04
曹正祥
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Nowadays, the development of new pesticides is more difficult, and the success rate of product development is also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of synthetic technique of acaricide emamectin benzoate, comprises the steps:

[0025] (1) Material mixing

[0026] Add isopropyl acetate to the reaction kettle, then add selective oxidation product, stir and mix evenly, add amination reagent and catalyst, stir and react at 20°C for 1h, the amination reagent is heptamethyldisilazane , the ratio of the isopropyl acetate, selective oxidation product, heptamethyldisilazane and catalyst is 1:1:1:0.4, and the catalyst is zinc trifluoroacetate;

[0027] (2) Ice bath reaction

[0028] Then the reaction product is dropped into the reaction still of ice-water bath, then add ethanol and sodium borohydride again, the time of reaction under described ice-water bath is 45min;

[0029] (3) Adjust the pH of the water layer

[0030] After the reaction, slowly add 5% glacial acetic acid aqueous solution to the reaction system, and adjust the pH of the water layer to 5;

[0031] (4) Remove the water layer

[0032] After adjust...

Embodiment 2

[0036] A kind of synthetic technique of acaricide emamectin benzoate, comprises the steps:

[0037] (1) Material mixing

[0038] Add isopropyl acetate to the reaction kettle, then add selective oxidation product, stir and mix evenly, add amination reagent and catalyst, stir and react at 23°C for 1.5h, the amination reagent is heptamethyldisilazide Alkane, the proportioning of described isopropyl acetate, selective oxidation product, heptamethyldisilazane and catalyst is 3:1:1:0.4, and described catalyst is zinc trifluoroacetate;

[0039] (2) Ice bath reaction

[0040] Then the reaction product is dropped into the reaction kettle of the ice-water bath, then ethanol and sodium borohydride are added, and the reaction time under the ice-water bath is 60min;

[0041] (3) Adjust the pH of the water layer

[0042] After the reaction, slowly add 10% glacial acetic acid aqueous solution to the reaction system, and adjust the pH of the water layer to 5.5;

[0043] (4) Remove the wat...

Embodiment 3

[0048] A kind of synthetic technique of acaricide emamectin benzoate, comprises the steps:

[0049] (1) Material mixing

[0050] Add isopropyl acetate to the reaction kettle, then add selective oxidation product, stir and mix evenly, add amination reagent and catalyst, stir and react at 26°C for 2h, the amination reagent is heptamethyldisilazane , the ratio of the isopropyl acetate, selective oxidation product, heptamethyldisilazane and catalyst is 4:1:1:0.4, and the catalyst is zinc trifluoroacetate;

[0051] (2) Ice bath reaction

[0052] Then the reaction product is dropped into the reactor of ice-water bath, then add ethanol and sodium borohydride, the time of reaction under the ice-water bath is 75min;

[0053] (3) Adjust the pH of the water layer

[0054] After the reaction, slowly add 15% glacial acetic acid aqueous solution to the reaction system, and adjust the pH of the water layer to 6;

[0055] (4) Remove the water layer

[0056] After adjusting the pH of the ...

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Abstract

The invention discloses a synthesis process of acaricide of emamectin benzoate. An animation reagent is heptamethyldisilazane, so that the reaction process is mild; meanwhile, the emamectin benzoate product yield is relatively high; isopropyl acetate, selective oxidation products, the heptamethyldisilazane and a catalyst are proportioned; the conversion rate of the reaction can be promoted; the catalyst is zinc trifluoroacetate. The emamectin benzoate product yield is ensured; meanwhile, the reaction implementation can be promoted; after the reaction, pressure reduction desolvation is performed; then, acetonitrile is used for recrystallization; a solvent of isopropyl acetate can be removed; the product purity is improved; after the emamectin benzoate is obtained, detection is performed by a high efficiency liquid chromatography method; the purity of the emamectin benzoate can be determined. The emamectin benzoate synthesized by the synthesis process has the advantages of high conversion rate and high purity; the market potential is great; the prospects are wide.

Description

technical field [0001] The invention belongs to the field of pesticide production methods, more specifically, the invention relates to a synthesis process of the acaricide emamectin benzoate. Background technique [0002] Nowadays, the development of new pesticides is difficult, and the success rate of product development is also low. Among many research methods, chemical modification of natural products or microbial fermentation products to obtain new pesticides has become one of the effective ways to develop new pesticides. Such pesticides are usually called biological source pesticides. Once on the market, bio-derived pesticides are known for their low toxicity, low residue, easy degradation, [0003] The advantages of being friendly to the environment are favored by people and have gained enough room for development. In the 1970s, abamectin, a biological fermentation product, attracted widespread attention because of its unique insecticidal mechanism, and was widely us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/00
CPCC07H17/08C07H1/00
Inventor 曹正祥
Owner 曹正祥