Tilmicosin phosphate preparation method

A technology of tilmicosin phosphate and phosphorylation, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as unstable product quality, low production efficiency, and incomplete amination, and achieve The effect of shortening the production cycle, reducing production costs and energy consumption, and easy operation

Active Publication Date: 2016-08-10
HUBEI LONGXIANG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is that after the tylosin fermentation liquid is pretreated, it undergoes formyl amination reduction, and then hydrolyzes to generate tilmicosin under acidic conditions, such as "A Synthetic Alternative Using Tylosin Fermentation Liquid" as disclosed in Chinese patent CN102659878A. The method of micosin and tilmicosin phosphate", the disadvantage of this preparation method is: because mycaminose has not been hydrolyzed and directly aminated, the steric hindrance effect leads to incomplete amination, and the impurities exceed the standard
[0005] In addition, at present, the spray drying method is mostly used in China to prepare the tilmicosin aqueous solution into tilmicosin phosphate, but the spray drying method has low production efficiency, expensive equipment, high cost and unstable product quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]①Put 130ml of purified water and 43g of tylosin tartrate into the reaction bottle, stir to dissolve, raise the temperature to 40°C, then add 20% sulfuric acid solution dropwise, adjust the pH value of the reaction solution to 1.5, and keep the solution at 40°C for 2 After 1 hour, add 120ml of butyl acetate, dropwise add 30% sodium hydroxide solution, adjust the pH value of the reaction solution to 10, stir for half an hour and let stand to separate layers, discard the water layer to obtain the organic layer;

[0042] ②Put 5.5g of 3,5-dimethylpiperidine into the organic layer, raise the temperature to 70°C, add dropwise a mixed solution of 25ml of ethyl acetate and 2.4g of formic acid, keep the reaction for 3 hours, cool down to 25°C, add 3.7 g phosphorus pentoxide, 1.4g of water was added dropwise, fully stirred and slowly solids were precipitated, stirred for 1 hour, after the precipitation was complete, centrifuged, vacuum-dried to obtain tilmicosin phosphate 39.9g, the...

Embodiment 2

[0044] ①Put 130ml of purified water and 43g of tylosin tartrate into the reaction bottle, stir to dissolve, heat up to 45°C, then add 20% sulfuric acid solution dropwise, adjust the pH value of the reaction solution to 1.7, and keep the solution at 45°C for 1.5 After 1 hour, add 110ml of butyl acetate, dropwise add 30% sodium hydroxide solution, adjust the pH value of the reaction solution to 11, stir for half an hour and let stand to separate layers, discard the water layer to obtain the organic layer;

[0045] ②Put 5.7g of 3,5-dimethylpiperidine into the organic layer, raise the temperature to 68°C, add dropwise a mixed solution of 30ml of ethyl acetate and 2.5g of formic acid, keep the reaction for 3 hours, cool down to 25°C, add 3.9 g phosphorus pentoxide, 1.5g of water was added dropwise, fully stirred and slowly solids were precipitated, stirred for 1 hour, after the precipitation was complete, centrifuged, vacuum-dried to obtain 40.2g of tilmicosin phosphate, the molar y...

Embodiment 3

[0047] ①Put 130ml of purified water and 43g of tylosin tartrate into the reaction bottle, stir to dissolve, heat up to 45°C, then add 20% sulfuric acid solution dropwise, adjust the pH value of the reaction solution to 1.9, and keep the solution at 45°C for 2 After 1 hour, add 110ml of butyl acetate, dropwise add 30% sodium hydroxide solution, adjust the pH value of the reaction solution to 11, stir for half an hour and let stand to separate layers, discard the water layer to obtain the organic layer;

[0048] ②Put 5.9g of 3,5-dimethylpiperidine into the organic layer, raise the temperature to 75°C, add dropwise a mixed solution of 30ml of ethyl acetate and 2.6g of formic acid, keep it warm for 2.5 hours, cool down to 25°C, and add 4g Phosphorus pentoxide, 1.5g of water was added dropwise, fully stirred and slowly solids were precipitated, stirred for 1 hour, after the precipitation was complete, centrifuged, vacuum dried to obtain 40.6g of tilmicosin phosphate, the molar yield...

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PUM

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Abstract

The invention relates to a tilmicosin phosphate preparation method. The preparation method comprises that through hydrolysis under acidic conditions, alkalization extraction, amination, phosphorylation with phosphoric pentoxide and a small amount of water, full stirring salification, centrifugation separation after solid precipitation and vacuum drying, tilmicosin phosphate is prepared from tylosin tartrate as a raw material. According to the preparation method, phosphoric pentoxide and a small amount of water are directly added into an amination liquid, the mixture undergoes a phosphorylation reaction and tilmicosin phosphate is precipitated from the organic solvent. The preparation method has a final mole yield of 95% or more and a simple process route, can be operated easily, is free of spray drying production equipment, has a low production cost and realizes recycle of an organic solvent.

Description

technical field [0001] The invention belongs to the field of veterinary medicine, and in particular relates to a preparation method of tilmicosin phosphate. Background technique [0002] Tilmicosin is a macrolide antibiotic developed by Elanco in the 1980s for livestock and poultry animals. As a widely used veterinary drug, tilmicosin not only has a strong inhibitory effect on all Gram-positive bacteria and some Gram-negative bacteria, spirochetes, etc., but also has a strong inhibitory effect on Actinobacillus pleuropneumoniae, Pasteurella, Pasteurella hemolytica and a variety of mycoplasma in livestock and poultry also have strong antibacterial activity. [0003] Tilmicosin is semi-synthesized from tylosin. Compared with tylosin, it has stronger antibacterial activity and better clinical application effect. [0004] At present, there are two main synthetic routes of domestic tilmicosin. One is that after the tylosin fermentation liquid is pretreated, it undergoes formyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/02
Inventor 陈清平王存亮许灵艳郭建武王铭宏
Owner HUBEI LONGXIANG PHARMA TECH CO LTD
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