Preparation method for tilmicosin phosphate

A technology of tilmicosin phosphate and tilmicosin, which is applied to the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., and can solve the problems of high product pretreatment requirements, long vacuum drying time, and unstable product quality and other problems, to achieve the effect of good product stability, simple method, and reduce equipment requirements

Inactive Publication Date: 2014-01-01
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both the spray drying method and the vacuum drying method have the following disadvantages: 1) high cost, troublesome operation, high requirements for product pretreatment, and expensive equipment; 2) the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve the solid tilmicosin in acetone at a mass:volume ratio of 1:5, mix well, heat to the reflux temperature of acetone, dissolve the tilmicosin, and filter. Add concentration to the filtrate and be the phosphoric acid aqueous solution of 37%, after fully stirring for 1 hour, the solution is cooled to room temperature, slowly add butyl acetate dropwise while stirring, the amount of butyl acetate added dropwise is 4 times of the volume of acetone, at this time A large number of crystals precipitated, kept stirring for 1 hour until the crystallization was complete, centrifuged, the solid was rinsed twice with cold butyl acetate, and dried to obtain tilmicosin phosphate as a solid. Yield: 97%, purity, 99.1%.

Embodiment 2

[0026] Dissolve the solid tilmicosin in ethyl acetate at a mass:volume ratio of 1:5, mix well, heat to the reflux temperature of ethyl acetate, dissolve the tilmicosin, and filter. Add concentration to the filtrate and be the phosphoric acid aqueous solution of 40%, after fully stirring for 2 hours, the solution is cooled to room temperature, slowly drop sherwood oil while stirring, the amount of dropwise sherwood oil is 5 times of ethyl acetate volume, at this moment A large number of crystals were precipitated, kept stirring for 1 hour until the crystallization was complete, then centrifuged, the solid was rinsed twice with cold petroleum ether, and dried to obtain tilmicosin phosphate as a solid. Yield: 95%, purity, 98.7%.

Embodiment 3

[0028] Dissolve the tilmicosin solid in methanol at a mass:volume ratio of 1:7, mix thoroughly, heat to the reflux temperature of methanol, dissolve the tilmicosin, and filter. In the filtrate, add a phosphoric acid aqueous solution with a concentration of 37%, and after fully stirring for 1 hour, the solution is cooled to room temperature, and diethyl ether is slowly added dropwise while stirring, and the amount of diethyl ether added dropwise is 5 times the volume of methanol. Keep stirring for 1 hour until the crystallization is complete, centrifuge, rinse the solid with cold ether twice, and dry to obtain tilmicosin phosphate as a solid. Yield: 96.5%, purity, 97.9%.

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PUM

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Abstract

The invention relates to a preparation method for tilmicosin phosphate. The preparation method for the tilmicosin phosphate comprises the following steps: completely mixing a tilmicosin solid and an organic solvent I; heating, dissolving and filtering; adding a phosphoric acid aqueous solution into filtration; completely stirring till the solution is salified; cooling to room temperature, slowly adding an organic solvent II dropwise while stirring till complete crystallization, and performing centrifugal separation; performing drip washing on the solid by using the cold organic solvent II for 2 to 3 times; drying the solid to obtain a tilmicosin phosphate solid. According to the preparation method of the tilmicosin phosphate, the tilmicosin is dissolved into solvents such as methanol, ethanol, acetone, dichloromethane and ethyl acetate and then is salified together with phosphoric acid in the organic solvent, so the aims of removing insoluble impurities and purifying products are realized and water-soluble impurities in the products are avoided; crystallization is performed according to different solubility of the tilmicosin phosphate in solvents such as butyl acetate, ethyl ether or petroleum ether to prepare the tilmicosin phosphate solid, so that the method is simple and convenient, and easy to operate; production is realized easily, the final yield reaches above 90 percent, and the purity reaches above 97 percent.

Description

technical field [0001] The invention relates to the technical field of biopharmaceuticals, in particular to a preparation method of tilmicosin phosphate. Background technique [0002] Tilmicosin is a chemical semi-synthetic macrolide antibiotic. It is a new type of drug specially used for animals. It has a wide antibacterial spectrum and has a strong inhibitory effect on Gram-negative bacteria and positive bacteria. And spirochetes also have a strong inhibitory effect. Clinically, it is mainly used for respiratory diseases caused by Actinomyces pleuropneumoniae, Pasteurella hemolytica, Pasteurella multocida, and livestock and poultry bodies. [0003] At present, the preparation of tilmicosin phosphate adopts the hydrolysis of tylosin in acid to obtain its hydrolyzed product descarbamose tylosin, which is then reacted with 3,5-dimethylpiperidine to obtain tilmic acid after alkalization. Cosin, then dissolve tilmicosin in phosphoric acid aqueous solution and spray dry to obt...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
Inventor 王义周丽娜王彬
Owner 宁夏泰瑞制药股份有限公司
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