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Gamithromycin crystal form I and preparation method thereof

A technology of gamimycin and its crystal form, which is applied in the field of gamimycin crystal form I and its preparation, can solve the problem of solubility and other physical and chemical properties, drug leached substances and differences in bioavailability, and can not meet the requirements of gamimycin crystal form Requirements, affecting drug stability, bioavailability and other issues, to achieve the effect of low preparation cost, easy control and easy preparation

Active Publication Date: 2015-07-22
QILU SYNVA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the development of gamimycin is mainly concentrated on the synthesis of gamimycin, and there is less research on the crystal form of gamimycin, and the control of the preparation process and the optimization of the preparation method are lacking, which has led to the development of the drug. There are differences in physical and chemical properties such as solubility, drug leachables, and biological effectiveness, which in turn affect the stability and bioavailability of the drug, and cannot meet the requirements of the veterinary drug industry for the crystal form of gamithromycin

Method used

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  • Gamithromycin crystal form I and preparation method thereof
  • Gamithromycin crystal form I and preparation method thereof
  • Gamithromycin crystal form I and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] At 60°C, add 10 g of gamimycin to a 500 ml three-neck flask, add 50 ml of isopropyl acetate, stir until the gaminomycin is completely dissolved, and then slowly add 200 ml of n-heptane dropwise. After the dropwise addition was completed, the temperature was lowered to 25°C and the crystal was grown with stirring for 2 hours, then filtered under reduced pressure, the filter cake was washed with 30ml of n-heptane, and vacuum-dried at 60°C for 24 hours to obtain a white crystalline powder, namely Gamithycin crystal Form I, the yield is 90%.

[0039] The X-ray powder diffraction pattern of gamimycin crystal form I was measured by X-ray diffractometer of PANalytical EMPYREAN in the Netherlands, the test conditions: Cu-Ka ray, 40kV, 40mA, the results are as follows figure 1 As shown, the values ​​of the characteristic peaks in the figure are shown in Table 1:

[0040] Table 1 The characteristic peak data of the X-ray powder diffraction pattern of gamithromycin crystal form Ⅰ...

Embodiment 2

[0048] At 60°C, add 10 g of gamimycin to a 500 ml three-necked flask, add 50 ml of ethyl acetate, stir until the gaminomycin is completely dissolved, and then slowly add 200 ml of n-heptane dropwise. After the dropwise addition was completed, the temperature was lowered to 25°C and the crystal was grown with stirring for 2 hours, then filtered under reduced pressure, the filter cake was washed with 30ml of n-heptane, and vacuum-dried at 60°C for 24 hours to obtain a white crystalline powder, namely Gamithycin crystal Form I, the yield is 85%.

[0049] There is no significant difference between the analysis results of gamimycin crystal form I prepared in Example 2 and the analysis results of gaminomycin crystal form I prepared in Example 1, wherein the characteristic absorption peaks of X-ray powder diffraction are 6.9681 °, 9.6321°, 10.2441°, 11.5745°, 13.0410°, 14.9921°, 19.2893°, 20.5751°, the stable gamithromycin crystal form I can be obtained repeatedly.

Embodiment 3

[0051] Under the condition of reflux at 90°C, add 10 g of gamimycin to a 500 ml three-necked flask, add 30 ml of ethyl acetate, stir until the gaminomycin is completely dissolved, and then slowly dropwise add it into 300 ml of n-heptane. After the dropwise addition was completed, the temperature was lowered to 25°C and the crystal was grown with stirring for 2 hours, then filtered under reduced pressure, the filter cake was washed with 30ml of n-heptane, and vacuum-dried at 60°C for 24 hours to obtain a white crystalline powder, namely Gamithycin crystal Form I, the yield was 94%.

[0052] The analysis results of the gamimycin crystal form I prepared in Example 3 are not significantly different from the analysis results of the gaminomycin crystal form I prepared in Example 1, wherein the characteristic absorption peaks of X-ray powder diffraction are 6.9652°, 9.6923°, 10.2368°, 11.6158°, 13.1116°, 15.0990°, 19.2642°, 20.5393°, the stable gamithromycin crystal form I can be obt...

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Abstract

The invention relates to a gamithromycin crystal form I and a preparation method thereof. According to the gamithromycin crystal form I, Cu-Ka radiation is used, X-ray powder diffraction shown by an angle 2(theta) is carried out, and the gamithromycin crystal form I has characteristic absorption peaks at 6.8165 degrees + / - 0.3 degree, 9.5249 degrees + / - 0.3 degree, 10.1349 degrees + / - 0.3 degree, 11.4490 degrees + / - 0.3 degree, 12.9373 degrees + / - 0.3 degree, 14.9831 degrees + / - 0.3 degree, 19.2302 degrees + / - 0.3 degree and 20.5137 + / - 0.3 degree. The gamithromycin crystal form I provided by the invention is easy to prepare, and related test data shows that the gamithromycin crystal form I is high purity, low in impurity content and good in stability.

Description

technical field [0001] The invention relates to gamimycin crystal form I and a preparation method thereof, belonging to the technical field of veterinary drug preparation. Background technique [0002] Gamithromycin belongs to the azalide subclass of 15-membered semi-synthetic macrolide antibiotics, it is an azalide, 15-membered ring semi-synthetic macrolide antibiotics, the 7a position of the lactone ring Nitrogen substituted by an alkyl group with a unique position, its structural formula is shown in formula (I). Due to its unique molecular structure, gamithromycin can selectively bind to the 50S subunit of bacterial ribosomes and stimulate the dissociation of peptidyl tRNA from ribosomes during translocation, thereby preventing peptide chain elongation and inhibiting its essential protein biosynthesis , eventually leading to bacterial death. It has the characteristics of wide antibacterial spectrum, strong antibacterial activity, excellent pharmacokinetic characteristic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/06
CPCC07B2200/13C07H1/06C07H17/00
Inventor 苏玉辉王秀龙刘雷刘全才孔梅吴连勇
Owner QILU SYNVA PHARMA
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