Preparation method of malic acid and tilmicosin compound salt

A technology of tilmicosin and malic acid, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of increasing the use cost, reducing the curative effect of diseases, complex preparation process, etc., and achieves easy operation, The effect of good water solubility and simple process route

Inactive Publication Date: 2017-05-31
SOUTHWEST UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve this problem in the prior art, the use of expensive special solvents has greatly increased its use cost
Although there have been reports on the preparation of new technologies such as nanoemulsions, liposomes, and soluble powders in recent years, their clinical application has been largely limited due to their complex preparation process and poor preparation stability.
Its phosphate is commonly used in veterinary clinics, but because of the poor palatability of existing tilmicosin phosphate preparations, it affects animals foraging, thereby reducing the curative effect on diseases

Method used

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  • Preparation method of malic acid and tilmicosin compound salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Put 0.67g of malic acid and 50ml of acetone in a 250ml three-neck flask, and under anhydrous conditions, stir and heat in an oil bath at 56°C for 10min to dissolve malic acid in acetone;

[0027] (2) equimolar tilmicosin crude drug 4.35g is dissolved in 30ml acetone, dissolves under anhydrous condition, makes the acetone solution of tilmicosin;

[0028] (3) The acetone solution of tilmicosin is transferred to the Soxhlet extractor, and the beaker is cleaned in stages with 10ml of acetone, and the washing solution is incorporated into the Soxhlet extractor; the Soxhlet extractor is connected to the side port of the three-necked flask, The middle port of the three-necked flask is connected to a condenser (to ensure no water), and the end of the condenser is connected to a drier (to prevent water in the air from entering). After the oil bath is heated to 56 ° C, under anhydrous conditions, the acetone of tilmicosin The solution was slowly dripped into the acetone solut...

Embodiment 2

[0032] (1) Put 0.67g of malic acid and 50ml of dichloromethane in a 250ml three-neck flask, and under anhydrous conditions, stir and heat in an oil bath at 50°C for 10 minutes to dissolve malic acid in dichloromethane;

[0033] (2) Equimolar tilmicosin crude drug 4.35g is dissolved in 30ml dichloromethane, dissolves under anhydrous condition, makes the dichloromethane solution of tilmicosin;

[0034] (3) Transfer the dichloromethane solution of tilmicosin to the Soxhlet extractor, wash the beaker with 10ml of dichloromethane in stages, and incorporate the washing solution into the Soxhlet extractor; connect the Soxhlet extractor to the three-necked flask On the side port of the three-neck flask, the middle port of the three-neck flask is connected to the condenser (to ensure that there is no water), and the end of the condenser is connected to the dryer (to prevent the water in the air from entering). The dichloromethane solution of Coxin is slowly dropped into the dichloromet...

Embodiment 3

[0037] (1) Dissolve 0.67g of malic acid in 50ml of ethyl acetate, stir and heat to dissolve in an oil bath at 60°C for 10min under anhydrous conditions, to obtain an ethyl acetate solution of malic acid;

[0038] (2) Equimolar tilmicosin crude drug 4.35g is dissolved in 50ml ethyl acetate, dissolves under anhydrous condition, makes the ethyl acetate solution of tilmicosin;

[0039] (3) Place the ethyl acetate solution of tilmicosin in a 250ml three-necked flask, add a stirrer, fix it in a constant temperature magnetic stirrer, connect the three-necked flask to the condensing device, and fill it with the tail gas of anhydrous calcium chloride Processing device, a dropping funnel filled with ethyl acetate solution of malic acid; after the oil bath is heated to 70°C, under anhydrous conditions, adjust the dropping speed of the dropping funnel, and add the ethyl acetate solution of malic acid to Slowly drop 0.5ml / min into the ethyl acetate solution of tilmicosin for reaction; afte...

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Abstract

The invention discloses a preparation method of malic acid and tilmicosin compound salt. The preparation method comprises the following steps of (1) dissolving the malic acid into an organic solvent, stirring, and heating and dissolving under the anhydrous condition, so as to prepare an organic solution of the malic acid; (2) dissolving crude drug of tilmicosin which is equimolar with the malic acid into the organic solvent, and dissolving under the anhydrous condition, so as to prepare an organic solution of the tilmicosin; (3) mixing the organic solution of the malic acid and the organic solution of the tilmicosin, heating to react under the anhydrous condition, controlling the reaction temperature to 50 to 70 DEG C, cooling a reaction liquid after reaction is complete, filtering the undissolved matter, performing rotary evaporation on filtrate, and recycling the organic solvent, so as to obtain a solid product, namely the malic acid and tilmicosin compound salt. The preparation method has the advantages that the technology is simple, the production cost is low, the water dissolvability of the prepared malic acid and tilmicosin compound salt is good, the dissolvability is good, the preparation property is good, and the mouth feel is proper.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a preparation method of tilmicosin malate double salt. Background technique [0002] Tilmicosin is a special macrolide antibiotic for poultry and animals. It was successfully developed by Elanco Animal Health Products Company in the UK in the 1980s. Tilmicosin is generally semi-synthesized from tylosin and has the same It has a similar antibacterial spectrum to gram-positive bacteria and some gram-negative bacteria, mold-type bacteria, spirochetes, etc., especially against Actinobacillus pleuropneumoniae, Pasteurella and animal mold-type bacteria. Tylosin has stronger antibacterial activity, and there is no cross-resistance with other antibiotics commonly used in clinic. [0003] Tilmicosin has a macrocyclic lactone structure, and the hydroxyl group on the ring is linked with sugar or substituted sugar in the form of glycosidic bonds, which reduces the tension of the ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/00
CPCC07H1/00C07H17/08
Inventor 李逐波刘禹嘉李德娟葛如兴
Owner SOUTHWEST UNIV
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