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Tildipirosin hexamethylene compound and preparation method

A new technology of solvent compound and Tiderol, which is applied in the preparation of sugar derivatives, organic chemical methods, chemical instruments and methods, etc., can solve the problems of small particles, easy aggregation, poor fluidity, etc.

Active Publication Date: 2016-11-09
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The new preparation process of tedilol reported in the patent is all needle-shaped, and the particles are very small and easy to coalesce, resulting in poor fluidity

Method used

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  • Tildipirosin hexamethylene compound and preparation method
  • Tildipirosin hexamethylene compound and preparation method
  • Tildipirosin hexamethylene compound and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of Tedirosine Cyclohexane Solvent Compound

[0027] Keep the temperature constant at 20°C, add 30g of cyclohexane into the crystallizer, add 6g of Tidelotide raw material into the solution, after adding the raw material, the system will have a solid suspension, continue to stir for 2 hours, filter the product, and place it in a 70°C drying oven Dry under normal pressure for 4 hours to obtain the final product. The powder diffraction pattern of the analysis product is as attached figure 1 As shown, the spectrum starts at 2θ=5.14 ° and the strongest peak; the specific data is shown in the following table:

[0028]

[0029]

[0030] The results of thermogravimetric analysis of the samples are attached figure 2 As shown, the weight loss is 8.4%, indicating that what is obtained is the tedirosine cyclohexane solvent compound; the scanning electron microscope SEM photo of the product is as attached image 3 As shown, it is rod-shaped.

Embodiment 2

[0032] Preparation of Tedirosine Cyclohexane Solvent Compound

[0033] Keep the temperature at 60°C, add 45g of cyclohexane and 15g of Tidelotol new raw materials into the crystallizer at one time, stir to make the system in a uniform suspension state, filter the white solid after 0.5h, filter the product, and place it in a 60°C drying oven under normal pressure Dry for 4h to get the final product. Analyze the powder diffraction pattern of the product and the attached figure 1 The spectrum has the same peak spectrum position and shape, and the spectrum is at 2θ=5.1 ° initial peak and the strongest peak; thermogravimetric analysis is as attached Figure 4 Shown, weight loss is 10.8%, what illustrate to obtain is tedirosine cyclohexane solvent compound; Product is observed under microscope and attached image 3 Similar, rod-shaped.

Embodiment 3

[0035] Preparation of Tedirosine Cyclohexane Solvent Compound

[0036] Keep the temperature at 30°C, add 40g of cyclohexane and 4g of Tidelotol new raw materials into the crystallizer at one time, stir to make the system in a uniform suspension state, filter the white solid after 4h, filter the product, and place it in a 65°C drying oven to dry under normal pressure 5h to obtain the final product. Analyze the powder diffraction pattern of the product and the attached figure 1 The spectrum has the same peak spectrum position and shape, and the spectrum is at 2θ=5.1 °. The initial peak and the strongest peak; the thermogravimetric analysis results show that the weight loss is 9.4%, indicating that what is obtained is the tedirosine cyclohexane solvent compound; the product is under the microscope Observation and Attachment image 3 Similar, rod-shaped.

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PUM

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Abstract

The invention relates to a Tildipirosin hexamethylene compound and a preparation method. Characteristic peaks exist in an X-ray powder diffraction spectrum at diffraction angles 2 theta which is 4.94-5.34, 6.58-6.98, 7.68-8.08, 8.46-8.86, 10.44-10.84, 10.86-11.26, 12.06-12.46, 13.04-13.44, 13.72-14.12, 14.30-14.70, 15.98-16.38, 16.62-17.02, 17.08-17.48, 17.74-18.14, 18.50-18.90, 18.94-19.34, 19.68-20.08, 20.10-20.50, 20.54-20.94, 21.38-21.78 and the like. The preparation method is simple, and the Tildipirosin hexamethylene compound can be prepared by a constant temperature suspension crystal transition method or a cooling crystallisation method, obtained products are stick-shaped, have complete crystal habit and are uniform in particle size.

Description

technical field [0001] The invention belongs to the field of medical technology and preparation of veterinary antibiotics, and in particular relates to 20,23-dipiperidinyl-5-O-mycaminosyl-tylonolide (also known as Tedirosin) cyclohexane solvent Compounds and methods for their crystallization. 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 the applied patent WO 2008012343 introduced a synthesis method for it. In March 2011, the European Union approved the marketing of a sterile injection with Tedirosin as the main component. [0003] The polymorphism of the drug will directly affe...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07B2200/13C07H1/06C07H17/08
Inventor 龚俊波吴送姑何林华向毅陈小林侯宝红曹建东
Owner TIANJIN UNIV
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