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Pseudo-polymorph of Arbekacin hydrochloride and preparation method and application thereof

A technology of pseudopolymorph and arbekacin, applied in the application field of arbekacin free base, can solve the problems of poor solid crystal form, inconvenient operation, limited purification effect, etc., and achieve thermodynamic stability and good crystal form , better purification effect

Inactive Publication Date: 2019-11-22
CHANGZHOU FANGYUAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is inconvenient to operate, the purification effect is limited, and the solid crystal form is poor
[0007] CN103826611A mentions arbekacin hydrochloride, but does not mention its preparation method and crystal form, nor does it mention its application in the production of high-purity arbekacin free alkali
Other domestic and foreign patents have not found reports of polymorphic forms of this compound

Method used

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  • Pseudo-polymorph of Arbekacin hydrochloride and preparation method and application thereof
  • Pseudo-polymorph of Arbekacin hydrochloride and preparation method and application thereof
  • Pseudo-polymorph of Arbekacin hydrochloride and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 5 g of arbekacin free base was dissolved in 15 mL of water and added to the reaction kettle. Add 6 mol / L hydrochloric acid aqueous solution dropwise to the reactor to adjust the final pH of the mother liquor to 3.0, and maintain the temperature at 30°C under stirring. Then add 100mL ethanol to the reaction kettle. After stirring for 3 hours, it was filtered to obtain 5.8 g of dry solid powder. The dried product was subjected to X-ray powder diffraction ( figure 1 ), DSC spectrum ( figure 2 ) and TGA spectrum ( image 3 ) was identified as pseudopolymorph II. The polymorph appears to have 2θ° of about 7.6, 9.6, 10.2, 11.5, 14.0, 14.5, 15.1, 16.3, 17.3, 19.3, 19.7, 20.0, 23.0, 23.4, 25.0, 25.3, 26.1, 27.0, 28.1, 28.9 , 33.2, 35.6, 37.2, 38.6, 39.0, 40.0, 41.0, 42.3, 43.3 and the X-ray powder diffraction pattern of the characteristic peaks represented by 45.5, such as figure 1 shown. The melting point of the pseudopolymorph II was measured to be 80-100°C.

Embodiment 2

[0041] 5 g of arbekacin free base was dissolved in 10 mL of water and added to the reaction kettle. Add 6 mol / L hydrochloric acid aqueous solution dropwise to the reaction kettle, adjust the final pH of the mother liquor to 4.0, and maintain the temperature at 30°C under stirring. Then add 70mL ethanol to the reaction kettle. After stirring for 3 hours, it was filtered to obtain 6.0 g of dry solid powder. The dried product was confirmed as pseudopolymorph II by X-ray powder diffraction, DSC spectrum and TGA spectrum.

Embodiment 3

[0043] 5 g of arbekacin free base was dissolved in 15 mL of water and added to the reaction kettle. Add 6 mol / L hydrochloric acid aqueous solution dropwise to the reaction kettle, adjust the final pH of the mother liquor to 4.5, and maintain the temperature at 30°C under stirring. 100 mL of methanol was then added to the reaction kettle. After stirring for 3 hours, it was filtered to obtain 5.7 g of dry solid powder. The dried product was confirmed as pseudopolymorph II by X-ray powder diffraction, DSC spectrum and TGA spectrum.

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Abstract

The invention discloses a pseudo-polymorph of Arbekacin hydrochloride and a preparation method and application thereof. The polymorph II shows an X-ray powder diffraction pattern of characteristic peaks with 2theta of 7.6+ / -0.2, 9.6+ / -0.2, 10.2+ / -0.2, 11.5+ / -0.2, 14.0+ / -0. 2, 14.5+ / -0.2, 15.1+ / -0.2, 16.3+ / -0.2, 17.3+ / -0.2, 19.3+ / -0.2, 19.7+ / -0.2, 20.0+ / -0.2, 23.0+ / -0.2, 23.4+ / -0.2, 25.0+ / -0.2, 25.3+ / -0.2, 26.1+ / -0.2, 27. 0+ / -0.2, 28.1+ / -0.2, 28.9+ / -0.2, 33.2+ / -0.2, 35.6+ / -0.2, 37.2+ / -0.2, 38.6+ / -0.2, 39.0+ / -0.2, 40.0+ / -0.2, 41.0+ / -0.2, 42.3+ / -0.2, 43.3+ / -0.2 and 45.5+ / -0.2 degrees.

Description

technical field [0001] The present invention relates to a novel pseudopolymorph II of arbekacin hydrochloride, a process for its preparation and its use in the production of high-purity arbekacin free base. Background technique [0002] Arbekacin (free base) is a compound having the following structure, and its sulfate salt is used in the treatment of pneumonia and sepsis caused by methicillin-resistant Staphylococcus aureus. [0003] [0004] Usually, arbekacin sulfate is obtained by using arbekacin free base synthesized according to the method described in Japanese Publication No. 52-33629 (Patent Document 1), and adding sulfuric acid to an aqueous solution of the arbekacin free base. , followed by freeze-drying and thus obtained in the form of a solid. In this case, the synthesized arbekacin free base was purified by chromatography. However, in order to improve the purification effect, a large amount of resin is usually required, the concentration of the eluent needs...

Claims

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Application Information

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IPC IPC(8): C07H15/234C07H1/06
CPCC07H15/234C07H1/06C07B2200/13
Inventor 王凯王海东丁顺戴俊蔡振一
Owner CHANGZHOU FANGYUAN PHARMA
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