Method of purifying nemadectin through crystallization

A purification method and nimoctin technology, applied in the direction of organic chemistry and the like, can solve the problems of being unsuitable for industrial production, serious environmental pollution, and high production costs, achieving simple and uncomplicated procedures, cheap and easy-to-obtain solvents, and reduced production costs. Effect

Active Publication Date: 2016-10-26
江苏海阔生物医药有限公司 +1
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  • Application Information

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Problems solved by technology

This method is not suitable for industrial production because of the use of high-priced mixe...

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  • Method of purifying nemadectin through crystallization

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Embodiment 1

[0038] Take 20.0 g of crude nimoctine, add 150 g of cyclohexane, heat to 60° C., fully stir to dissolve, remove insoluble matter by suction filtration, and obtain nimoctine solution. Sampling was carried out for high-performance liquid phase detection, and the content of nimoctine was 12.9 grams. The nimoctine solution was kept at 60° C., the stirring speed was set to 12 rpm, n-heptane was slowly added dropwise until the solution became turbid, and nimoctine crystals were added as seeds. Then cool down to 20°C at a rate of 18°C / hour, stir until crystals are precipitated, keep at 20°C for 120 minutes, then cool down to 5°C at a rate of 8°C / hour, keep warm for 12 hours, stir once every 2 hours to suspend the crystals , to speed up nucleation and diffusion, and increase the growth rate of crystal nuclei. Finally, the wet crystals of nimoctine were filtered and vacuum-dried to obtain 11.5 grams of dry powder of nimoctine, which was tested by high performance liquid phase. The con...

Embodiment 2

[0040] Take 18.0 g of crude nimoctine, add 180 g of petroleum ether, heat to 65° C., fully stir to dissolve, remove insoluble matter by suction filtration, and obtain nimoctine solution. Sampling was carried out for high-performance liquid phase detection, and the content of nimoctine was 11.8 grams. The nimoctine solution described in step (1) was kept at 65° C., the stirring speed was set to 15 rpm, methylcyclohexane was slowly added dropwise until the solution became turbid, and nimoctine crystals were added as seed crystals. Then cool down to 15°C at a rate of 15°C / hour, stir until crystals precipitate, keep at 15°C for 60 minutes, then cool down to 8°C at a rate of 5°C / hour, keep warm for 12 hours, stir once every 2 hours to suspend the crystals , to speed up nucleation and diffusion, and increase the growth rate of crystal nuclei. Finally, the wet crystals of nimoctine were filtered and vacuum-dried to obtain 10.1 g of nimoctine dry powder. Sampling was carried out for...

Embodiment 3

[0042] Take 25.0 g of the crude product of nimoctine, add 50 g of benzene, heat to 58° C., fully stir to dissolve, remove the insoluble matter by suction filtration, and obtain the nimoctine solution. Sampling was carried out for high-performance liquid phase detection, and the content of nemoctine was 13.5 grams. The nemoctine solution was kept at 58° C., the stirring speed was set to 8 rpm, n-octane was slowly added dropwise until the solution became turbid, and nemoctine crystals were added as seed crystals. Then cool down to 25°C at a rate of 20°C / hour, stir until crystals are precipitated, keep at 25°C for 120 minutes, then cool down to 6°C at a rate of 7°C / hour, keep warm for 24 hours, stir once every 2 hours to suspend the crystals , to speed up nucleation and diffusion, and increase the growth rate of crystal nuclei. Finally, the wet crystals of nimoctine were filtered and vacuum-dried to obtain 11.5 grams of dry powder of nimoctine, which was tested by high performan...

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Abstract

The invention provides a method of purifying nemadectin through crystallization. The method includes: taking a nemadectin crude product, adding a first nonpolar solvent, and heating for dissolving to obtain a nemadectin solution; adding a second nonpolar solvent to be turbid, and performing gradient cooling for crystallization; sequentially filtering and drying to obtain a nemadectin pure product. By using the method, the problem that the nemadectin crude product is difficult to crystallize is solved, and high-purity nemadectin crystals are obtained. The method is simple to operate, simple in equipment, low in cost, environment-friendly and convenient for industrial production.

Description

technical field [0001] The invention relates to a method for purifying nemoctine through crystallization, belonging to the technical field of antibiotic purification. Background technique [0002] Nemoctine is a hexadecetone antibiotic produced by fermentation of Streptomyces blue gray, with a molecular weight of 612.8 and a chemical formula of C 36 h 52 o 8 , the appearance of high-purity finished products is off-white or light yellow. Nimoctine can be used to treat parasites inside and outside animals, and has the characteristics of broad insecticidal spectrum, easy degradation, low residue, and little environmental pollution. At present, nimoctine is mainly used for the synthesis of moxidectin with wider anthelmintic activity. During the synthesis process, the purity of nimoctine seriously affects the quality of finished moxidectin. Product quality is of particular importance. [0003] Due to the characteristics of nimoctine itself and the low purity during crystalli...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 贾坤周树林饶月亮吕祖平苗玉武王云德龚伟中
Owner 江苏海阔生物医药有限公司
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