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Tildipirosin 1,4-dioxane solvate and preparation method thereof

A solvent compound, a new technology of tedirox, applied in the preparation of sugar derivatives, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of dust, cumbersome process, high energy consumption, etc., to avoid coalescence and dust. Phenomenon, the effect of good particle fluidity and uniform particle size distribution

Active Publication Date: 2016-10-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The new crystalline form of tedrol prepared by the world patent WO2009 / 013351A2 is a long needle-shaped product, and the new solid powder of tedrol has a strong electrostatic effect, which leads to the phenomenon of dust in the production process
Moreover, the preparation of the new non-solvent or solvent compound in the above-mentioned patent is the cooling crystallization of high-temperature dissolution or high-temperature evaporation crystallization or dissolution evaporation crystallization.

Method used

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  • Tildipirosin 1,4-dioxane solvate and preparation method thereof
  • Tildipirosin 1,4-dioxane solvate and preparation method thereof
  • Tildipirosin 1,4-dioxane solvate and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0029] Preparation of tedirosin 1,4-dioxane solvent compound

[0030] At 20°C, add 40g of 1,4-dioxane into the crystallizer and stir to keep the system in a good mixing state. Add 4g of Tiderol new raw material into the crystallizer in four times, 1g each time, with an interval of 20 minutes between each addition, after adding the raw material, continue to stir the solution for 0.5h, filter the solid, and dry to obtain the product.

[0031] The product is subjected to X-ray powder analysis, and its diffraction pattern is as attached figure 1 As shown, the spectrum has initial peaks at 2θ=6.06° and 8.42°, and the strongest peak at 2θ=18.60. See the table below for specific data:

[0032]

[0033]

[0034] Carry out TGA thermogravimetric analysis to the product in this embodiment, thermogravimetric analysis is nitrogen purge environment, and heating rate is 10 ℃ / min, obtains analysis result curve as attached figure 2As shown, the heating weight loss temperature range ...

Embodiment 2

[0036] Preparation of tedirosin 1,4-dioxane solvent compound

[0037] Keep the temperature constant at 40°C, add 30g of 1,4-dioxane into the crystallizer, add and stir to keep the system in a good mixing state. Add 10g of Tiderol new raw material to the crystallizer in five times, 2g each time, and the interval between each addition is 40min. After adding the raw material, continue to stir the solution for 3h, filter the solid, 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=6.0° and 8.4°, and the strongest peak at 2θ=18.6°; TGA weight loss curve and attached figure 2 similar, with a loss of 10.9% in size, crystal shape and attached image 3 The same as a short rod.

Embodiment 3

[0039] Preparation of tedirosin 1,4-dioxane solvent compound

[0040] With a constant temperature of 30°C, add 35g of 1,4-dioxane into the crystallizer and stir to keep the system in a good mixing state. Add 5 g of the new raw material of Tiderol into the crystallizer in 3 times, with an interval of 30 minutes between each addition. After adding the raw material, continue to stir the solution for 1 hour, filter the solid, 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=6.0° and 8.4°, and the strongest peak at 2θ=18.6°; TGA weight loss curve and attached figure 2 similar, with a loss of 10.6% in size, crystal shape and attached image 3 Same as rod.

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Abstract

The invention provides a tildipirosin 1,4-dioxane solvate and a preparation method thereof. Characteristic peaks occur in an X-ray powder diffraction pattern represented by 2theta when 2theta is equal to 6.06+ / -0.2, 8.42+ / -0.2, 9.34+ / -0.2, 9.94+ / -0.2, 10.28+ / -0.2, 12.34+ / -0.2, 13.44+ / -0.2, 13.74+ / -0.2, 14.66+ / -0.2, 15.58+ / -0.2, 15.78+ / -0.2, 16.40+ / -0.2, 17.00+ / -0.2, 17.90+ / -0.2, 18.60+ / -0.2, 19.32+ / -0.2, 20.10+ / -0.2, 21.40+ / -0.2, 22.34+ / -0.2, 22.68+ / -0.2, 23.34+ / -0.2 and 24.18+ / -0.2. The preparation method employs a constant-temperature suspended crystal transformation process and is simple in process and low in energy consumption. The tildipirosin 1,4-dioxane solvate is in a rod shape and crystal is of a regular shape.

Description

technical field [0001] The invention belongs to the technical fields of medical technology and preparation of veterinary antibiotics, and in particular relates to a tedirosin 1,4-dioxane solvent compound and a preparation method thereof. Background technique [0002] Tedirosin, molecular formula C 41 h 71 N 3 0 8 , molecular weight: 734.03, chemical name is 20-deoxy-23-deoxy-5-oxo-[3,6-dideoxy-3-(dimethylamino)-D-glucopyranosyl] 20,23-dipiper Pyridyl Tylenolactone. Tedirosin belongs to the class of macrolides. Macrolides have long been known to be effective in the treatment of infectious diseases in humans, livestock, poultry and other animals. [0003] 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, Paste...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06C07D319/12
CPCC07B2200/13C07D319/12C07H1/06C07H17/08
Inventor 龚俊波吴送姑侯宝红尹秋响
Owner TIANJIN UNIV
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