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Refinement method of methylamino abamectin benzoate

A technology for methylamino abamectin and a purification method, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem of inability to achieve large-scale industrial production, inability to meet the needs of high-end preparations, and low product purity. problems, to facilitate large-scale industrial production, stable product quality, and improve the effect of purity

Active Publication Date: 2014-01-08
QILU SYNVA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The domestic and foreign content control standards of emamectin benzoate raw materials are basically below 70%, and the product purity is low, which cannot meet the needs of high-end preparations
When a small amount of high-purity products is required, silica gel column purification is used. This purification method is costly and cannot achieve large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for refining emamectin, the steps are as follows:

[0043] (1) Keep the temperature at 20°C to 25°C, add 200kg of emamectin into 800kg of acetonitrile, stir to dissolve. A mixed solution prepared by 17kg of phosphoric acid and 100kg of acetonitrile was added dropwise to the reaction solution, and the reaction was stirred for 0.5 to 1 hour. Add 2400 kg of toluene, stir and crystallize for 1 hour, cool down to -5°C to 5°C, stir for 5 to 6 hours, centrifuge, and wash the filter cake with toluene at -5°C to 5°C. Vacuum drying the product at 30°C to obtain emamectin phosphate 161kg, HPLC content 90.3%.

[0044] (2) Add 161kg of emamectin phosphate prepared in step (1) into 1932kg of water, and stir to dissolve. Add ethyl acetate 1127kg and stir evenly. Use 30wt% sodium hydroxide solution to adjust the pH value to 6.8, static layering for 1.5h, separate the organic phase, and concentrate in vacuo at 35-65°C to obtain 102kg of refined emamectin free base, with an H...

Embodiment 2

[0047] A method for refining emamectin, the steps are as follows:

[0048] (1) Keep the temperature at 20°C to 25°C, add 200kg of emamectin into 600kg of acetonitrile, stir to dissolve. A mixed solution of 28.3kg of phosphoric acid and 100kg of acetonitrile was added dropwise to the reaction solution, and the reaction was stirred for 0.5 to 1 hour. Add 2000 kg of toluene, stir and crystallize for 1 hour, cool down to -5°C to 5°C, stir for 5 to 6 hours, centrifuge, and wash the filter cake with toluene at -5°C to 5°C. Vacuum drying the product at 30° C. to obtain 165 kg of emamectin phosphate, with an HPLC content of 88.4%.

[0049] (2) Add 165kg of emamectin phosphate prepared in step (1) into 1650kg of water, and stir to dissolve. Add ethyl acetate 990kg and stir evenly. 30wt% concentration of sodium hydroxide solution to adjust the pH to 7, static layering for 1h, separation of the organic phase, 35 ~ 65 ° C vacuum concentration to obtain fine emamectin free base 110kg, HPL...

Embodiment 3

[0052] A method for refining emamectin, the steps are as follows:

[0053] (1) Keep the temperature at 20°C to 25°C, add 200kg of emamectin into 1000kg of acetonitrile, stir to dissolve. A mixed solution of 14.2kg of phosphoric acid and 100kg of acetonitrile was added dropwise to the reaction solution, and the reaction was stirred for 0.5 to 1 hour. Add 3000 kg of toluene, stir and crystallize for 1 hour, cool down to -5°C to 5°C, stir for 5 to 6 hours, centrifuge, and wash the filter cake with toluene at -5°C to 5°C. Vacuum drying the product at 30°C to obtain emamectin phosphate 158kg, HPLC content 90.4%.

[0054] (2) Add 158kg of emamectin phosphate prepared in step (1) into 2370kg of water, and stir to dissolve. Add ethyl acetate 1264kg and stir evenly. A 30wt% sodium hydroxide solution was used to adjust the pH to 7.5, and the layers were static for 2.5 hours. The organic phase was separated and concentrated in vacuo at 35-65° C. to obtain 109 kg of refined emamectin f...

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Abstract

The invention relates to a refinement method of methylamino abamectin benzoate. The refinement method comprises the following steps: carrying out dissolved clarification on methylamino abamectin serving as a raw material in a polar solvent A, then adding phosphoric acid, devitrifying in methylbenzene so as to obtain methylamino abamectin phosphate, dissolving with water, adding an ester solvent B, adjusting the pH value, standing still, layering, carrying out vacuum concentration so as to obtain high-quality methylamino abamectin free alkali, salifying the high-quality methylamino abamectin free alkali and benzoic acid in a methyl tertiary-butyl ether, thus obtaining the high-content methylamino abamectin benzoate. The refinement method is simple in process and can be used for realizing industrial large-scale production; and the product has high purity and is used for preparing high-end preparations.

Description

technical field [0001] The invention relates to a method for refining emamectin benzoate, which belongs to the technical field of pesticide raw materials. Background technique [0002] Emamectin benzoate (referred to as emamectin salt for short) is a new type of high-efficiency insecticide and acaricide synthesized by avermectin. It has extremely high biological activity especially against lepidopteran pests and has low toxicity. , less residue, no pollution and other characteristics, so it is widely used in agricultural production. [0003] Chinese patent document CN103012525A provides a method for synthesizing emamectin benzoate. First, abamectin is added to the dichloromethane solution, and at -20°C to -15°C, the compound Oxidation reagent, the obtained synchronous oxidation product, add heptamethyldisilazane, react at 0-40°C for 30min-90min, and obtain the intermediate of C4”=O that is selectively imidized; at -10°C~ Under the condition of 0°C, use ethanol as solvent a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 方明锋刘全才孟祥杰孔梅吴连勇
Owner QILU SYNVA PHARMA
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