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A kind of abamectin refining method

A technology of abamectin and a purification method, applied in the field of medicine, can solve the problems of large solvent consumption, cumbersome steps, and high product loss rate, and achieve the effects of saving production time and cost, eliminating oxidized impurities, and reducing the number of crystallization times.

Active Publication Date: 2022-08-02
江苏海岸药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current refining method of abamectin has high cost and is not suitable for industrial production, and the steps are cumbersome, the solvent consumption is large, the product loss rate is high, and the purity is low

Method used

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  • A kind of abamectin refining method
  • A kind of abamectin refining method
  • A kind of abamectin refining method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, take by weighing 15.0g abamectin crude product (purity 90.27%, oxidized impurity 4.19%) and join in the single-necked bottle of 100ml, in single-necked bottle, add 70ml isopropanol, single-necked bottle is placed in the oil of 85 ℃ Carry out stirring and dissolving in the bath pot to obtain the abamectin crude product solution, after the abamectin crude product solution is carried out the reflux reaction of 2h, slowly drip the formamide of 15ml into the described abamectin crude product solution species, then carry out 5h of Crystallization by cooling, suction filtration of the crude Abamectin solution to obtain a solid, and vacuum drying of the solid at 50° C. to obtain a pure Abamectin product.

[0042] Use high performance liquid chromatography to analyze the crude Abamectin and the pure Abamectin obtained, please refer to Table 1, Abamectin B1a 13.61g, yield 90.73%, purity 92.86%, oxidized impurities 2.18%.

[0043] Table 1

[0044]

[0045]

Embodiment 2

[0046] Embodiment 2, take by weighing the pure Abamectin product among the 8.0g embodiment 1 and join in the single-neck bottle of 100ml as Abamectin crude product (purity 92.86%, oxidation impurity 2.18%), in the single-neck bottle, add 80ml ethanol , the single-necked bottle was placed in an oil bath at 85°C for stirring and dissolving to obtain the abamectin crude product solution, after the abamectin crude product solution was subjected to a reflux reaction for 1.5h, 10ml was slowly added dropwise to the abamectin crude product solution. formamide, followed by cooling and crystallization for 3 hours, suction filtration of the crude Abamectin solution to obtain a solid, and vacuum drying of the solid at 50°C to obtain pure Abamectin.

[0047] The obtained pure abamectin was analyzed by high performance liquid chromatography, please refer to Table 2, and 7.53 g of abamectin B1a was obtained, the yield was 94.13%, the purity was 94.95%, and the oxidized impurity was 0.48%.

...

Embodiment 3

[0050] Embodiment 3, take by weighing 8.8g Abamectin crude product (purity 94.63%, oxidized impurity 0.18%) and join in the single-necked bottle of 100ml, add 70ml ethanol, the single-necked bottle is placed in the oil bath pot of 85 ℃, stirring and dissolving obtains Abamectin crude product solution, after the abamectin crude product solution is subjected to reflux reaction for 1h, slowly add 35ml of formamide to the abamectin crude product solution, carry out cooling crystallization for 3h, to the abamectin crude product solution Suction filtration was performed to obtain a solid, and the solid was vacuum-dried at 50° C. to obtain pure abamectin.

[0051]Use high performance liquid chromatography to analyze the crude Abamectin and the pure Abamectin obtained, please refer to Table 3, obtain Abamectin B1a 8.14g, yield 92.50%, purity 94.92%, oxidized Impurities 0.02%.

[0052] table 3

[0053]

[0054]

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Abstract

The invention discloses a method for purifying abamectin, comprising step 1: adding crude abamectin into a solvent, heating and stirring in an oil bath to dissolve to obtain a crude abamectin solution, the The mass volume ratio of abamectin crude product and described solvent is 1:(4-10), unit g / ml; Step 2: the abamectin crude product solution is carried out the reflux reaction of 1h-2h; Step 3: to step Formamide was added to the crude Abamectin solution that had undergone reflux reaction in the second, cooling and crystallization was carried out, suction filtration was performed to obtain a solid, and the solid was vacuum-dried to obtain a pure Abamectin product. The crystallization times are few, the yield is high, and the oxidation impurities are effectively eliminated.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a method for refining abamectin. Background technique [0002] Abamectin, also known as avermectin, is a macrolide antibiotic with 16-membered ring structure produced by the fermentation of Streptomyces avermectin. It has the characteristics of agriculture, animal husbandry and medicine. It has strong anthelmintic and insecticidal activities, and is widely used in the treatment of various internal and external parasitic diseases of livestock. Abamectin is easily degraded under natural conditions, safe for humans and animals, and has little impact on natural enemies. It belongs to green biological pesticides. However, the quality of Abamectin produced by various manufacturers is quite different, which has a great impact on the subsequent synthesis of derivatives. How to improve the crystallization method of abamectin and ensure the quality of the product is a problem to be solv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/06C07H17/08
CPCC07H1/06C07H17/08
Inventor 牟英波郭妞缪世峰
Owner 江苏海岸药业有限公司
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