Tildipirosin acetone solvent compound and preparation method

A technology of tediloxine and acetone solvent, which is applied in the fields of medical technology and veterinary antibiotic preparation, can solve the problems of small bulk density, poor fluidity, coalescence and the like

Active Publication Date: 2016-10-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problems of new needle-like crystal habit, low bulk density, poor fluidity and agglomeration of tedrol in the prior art, and provide a new resource of tedrol

Method used

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  • Tildipirosin acetone solvent compound and preparation method
  • Tildipirosin acetone solvent compound and preparation method
  • Tildipirosin acetone solvent compound and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of tedirosine acetone solvent compound

[0026] Weigh 4g of acetone in the crystallizer, raise it to 40°C, then add 4g of amorphous Tedirosin to dissolve while stirring, lower it to 30°C at 0.1°C / min, continue to stir, and a large number of white blocky crystals appear , filtered and dried to obtain the product. Carry out X-ray powder diffraction analysis to the product, the graph is as attached figure 1 As shown, the spectra start peaks at 2θ=6.12° and 8.48°, and the strongest peak at 2θ=17.20. The specific data are as follows:

[0027]

[0028]

[0029] Carry out TGA thermogravimetric analysis on the product, the analysis is nitrogen purging environment, the heating rate is 10 ℃ / min, the analysis results are as attached figure 2 As shown, there is an obvious desolventization peak, and the desolvation weight loss percentage is 7.52%. The scanning electron microscope photo SEM of the product is attached image 3 The block is shown, indicating that...

Embodiment 2

[0031] Preparation of tedirosine acetone solvent compound

[0032] Add 3g of the new raw material of Tedirol with crystal form III in the crystallizer, then add 15g of acetone, keep the temperature at 55°C, and dissolve completely. Cool down to 10°C at 10°C / min to form white blocky crystals, filter and dry to obtain the product. X-ray powder diffraction pattern of the product and attached figure 1 Consistent, with the same peak spectrum position and shape, the relative intensity values ​​of the peaks are basically the same, the spectrum starts at 2θ=6.1° and 8.4°, and the strongest peak at 2θ=17.2; TGA weight loss curve and attached figure 2 similar, with a loss of 7.4% in size, crystal shape and attached image 3 The same is lumpy, indicating that what is obtained is tedirosine acetone solvent compound.

Embodiment 3

[0034] Preparation of tedirosine acetone solvent compound

[0035] Add 4g of Tidelotol new raw material into the crystallizer, then add 24g of acetone, keep the temperature at 52°C, and dissolve completely. The temperature was lowered to 5°C at 5°C / min to form white blocky crystals, which were filtered and dried to obtain the product. X-ray powder diffraction pattern of the product and attached figure 1 Consistent, with the same peak spectrum position and shape, the relative intensity values ​​of the peaks are basically the same, the spectrum starts at 2θ=6.1° and 8.4°, and the strongest peak at 2θ=17.2; TGA weight loss curve and attached figure 2 Similar, the weight loss was 7.38% in size, crystal shape and attached image 3The same is lumpy, indicating that what is obtained is tedirosine acetone solvent compound.

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Abstract

The invention relates to a Tildipirosin acetone solvent compound and a preparation method. An X-ray powder diffraction spectrum of the Tildipirosin acetone solvent compound has characteristic peaks at a diffraction angle 2theta which is equal to 6.12 degrees plus or minus 0.2 degrees, 8.48 degrees plus or minus 0.2 degrees, 9.39 degrees plus or minus 0.2 degrees, 9.98 degrees plus or minus 0.2 degrees, 10.32 degrees plus or minus 0.2 degrees, 11.40 degrees plus or minus 0.2 degrees, 13.46 degrees plus or minus 0.2 degrees, 13.90 degrees plus or minus 0.2 degrees, 14.58 degrees plus or minus 0.2 degrees, 15.78 degrees plus or minus 0.2 degrees, 16.64 degrees plus or minus 0.2 degrees, 17.20 degrees plus or minus 0.2 degrees, 17.94 degrees plus or minus 0.2 degrees, 18.88 degrees plus or minus 0.2 degrees, 19.58 degrees plus or minus 0.2 degrees, 20.16 degrees plus or minus 0.2 degrees, 20.64 degrees plus or minus 0.2 degrees, 22.10 degrees plus or minus 0.2 degrees, 22.74 degrees plus or minus 0.2 degrees, 23.38 degrees plus or minus 0.2 degrees, 24.64 degrees plus or minus 0.2 degrees and 26.30 degrees plus or minus 0.2 degrees. The preparation method is simple, and a prepared product is block-shaped, has a complete crystal habit and has the characteristics of good fluidity, high bulk density and good stability.

Description

technical field [0001] The invention belongs to the field of medical technology and preparation of veterinary antibiotics, in particular to 20-deoxy-23-deoxy-5-oxo-[3,6-dideoxy-3-(dimethylamino)-D-glucopyranosyl ] 20,23-Dipiperidinyl Tylenolactone (hereinafter referred to as: Tedirosin) acetone solvent compound and its crystallization preparation method. Background technique [0002] Macrolides play an indispensable role in the treatment of the pathology of plethora, and have the characteristics of fast curative effect and high safety. Tedirosin is a safe and effective broad-spectrum antibiotic for the treatment of livestock and poultry respiratory infections caused by Mannheimia haemolytica, Pasteurella multocida and Haemophilus somnus. Tedirosin was developed by Intervet-Schering-Plough, and in March 2011 the European Union approved the marketing of Tedirosin injection. [0003] The polymorphism of the drug will directly affect the stability, solubility, bioavailability,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06C07C45/81C07C49/08
CPCC07B2200/13C07C45/81C07H1/06C07H17/08C07C49/08
Inventor 龚俊波吴送姑侯宝红杜世超
Owner TIANJIN UNIV
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