A kind of preparation method of tilmicosin phosphate

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...

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.