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Tilmicosin phosphate preparation method

A technology of tilmicosin phosphate and tilmicosin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high cost, long vacuum drying time, and great harm to human body, and achieve Reduce equipment requirements, good product stability, and reduce production costs

Inactive Publication Date: 2017-11-24
SHANDONG JIULONG HISINCE PHARMA CO LTD
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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 cannot be purified; 3) spray drying It is easy to produce a large amount of dust, which is harmful to the human body; 4) The vacuum drying time is long, the energy consumption is high and the product quality is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 50g of tilmicosin to 100g of purified water, raise the temperature to 35°C, add dropwise phosphoric acid to adjust the pH to 6.0, at this time the tilmicosin has been dissolved, filter, react at 38°C for 2 hours, cool to 0°C, drop Add 200g of tetrahydrofuran to completely precipitate tilmicosin phosphate, centrifuge and dry. The yield of the final product obtained was 96%, and the purity was 89.3%.

Embodiment 2

[0024] Add 50g of tilmicosin to 50g of purified water, raise the temperature to 30°C, add dropwise phosphoric acid to adjust the pH to 5.0, at this time the tilmicosin has been dissolved, filter, react at 35°C for 2 hours, cool down to 1°C, drop Add 50g of tetrahydrofuran to completely precipitate tilmicosin phosphate, centrifuge and dry. The yield of the final product obtained was 95.5%, and the purity was 89.0%.

Embodiment 3

[0026] Add 50g of tilmicosin to 500g of purified water, raise the temperature to 40°C, add dropwise phosphoric acid to adjust the pH to 8.0, at this time the tilmicosin has been dissolved, filter, react at 40°C for 2 hours, cool down to 0°C, drop Add 1000g of tetrahydrofuran to completely precipitate tilmicosin phosphate, centrifuge and dry. The yield of the final product obtained was 95.5%, and the purity was 89.2%.

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PUM

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Abstract

The invention relates to a tilmicosin phosphate preparation method, which comprises: adding tilmicosin to a certain proportion of purified water, heating, adding phosphoric acid in a dropwise manner to adjust the pH value so as to dissolve, filtering, cooling, adding a sedimentation agent to precipitate a crystal, carrying out centrifugation, and drying, wherein the obtained product is tilmicosin phosphate. According to the present invention, the preparation method has advantages of safety, environmental protection, good product quality and low cost, and can be used for industrial production; and the produced product has advantages of high purity and good stability.

Description

technical field [0001] The invention belongs 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): C07H1/00C07H17/08
Inventor 杨统鹏李志远殷习栋韩伟胡文婷刘丕雷宋晶晶
Owner SHANDONG JIULONG HISINCE PHARMA CO LTD
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