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Etimicin sulfate pseudo-polymorph, and preparation method and application thereof

A pseudopolymorphic, sulfate technology, applied in the preparation of sugar derivatives, chemical instruments and methods, medical preparations containing active ingredients, etc.

Active Publication Date: 2013-07-10
SHANGHAI INST OF PHARMA IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other domestic and foreign patents have not found reports of polymorphic forms of this compound

Method used

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  • Etimicin sulfate pseudo-polymorph, and preparation method and application thereof
  • Etimicin sulfate pseudo-polymorph, and preparation method and application thereof
  • Etimicin sulfate pseudo-polymorph, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0038] 2 g of 1-N-ethyl gentamicin C 1a Sulfate was dissolved in 10ml of water and added to the kettle. Then 30ml of methanol was added to the reaction kettle, and the temperature was maintained at 40°C under stirring. And add 4 mol / L aqueous sulfuric acid solution dropwise to the reactor to adjust the final pH of the mother liquor to 5.0. After stirring for 1 h, it was filtered to obtain 1.3 g of dry crystalline solid. The dried product was identified as pseudopolymorph I by X-ray powder diffraction, DSC spectrum and TGA spectrum. The polymorph I is shown to have 2θ° of about 5.1, 6.0, 7.0, 7.6, 8.5, 10.9, 12.5, 13.1, 13.7, 15.5, 16.0, 16.6, 17.2, 17.6, 19.4, 19.9, 20.1, 20.5, 21.7, The X-ray powder diffraction patterns of the characteristic peaks represented by 22.6, 23.2, 24.0, 24.5, 26.0, 26.7, 27.1, 27.6, 28.4 and 28.8 are shown in Figure 1. The melting point of this pseudopolymorph I was measured to be 114°C-133°C.

Embodiment 2

[0040] 6 g of 1-N-ethyl gentamicin C 1a Sulfate was dissolved in 10ml of water and added to the kettle. Then, 60 ml of methanol was added to the reaction kettle, and the temperature was maintained at 40° C. under stirring. And add dropwise 4mol / L aqueous sulfuric acid solution to the reactor to adjust the final pH of the mother liquor to 4.5. After stirring for 1 h, it was filtered to obtain 7.5 g of dry crystalline solid. The dry product was analyzed by X-ray powder diffraction ( Figure 1A ), DSC spectrum ( figure 2 upper solid line) and TGA spectrum ( image 3 ) was identified as pseudopolymorph I. The melting point of this pseudopolymorph I was measured to be 114°C-133°C.

Embodiment 3

[0042] 6 g of 1-N-ethyl gentamicin C 1a Sulfate was dissolved in 10ml of water and added to the kettle. Then 20ml of ethanol was added to the reaction kettle, and the temperature was maintained at 60°C under stirring. And add 6 mol / L aqueous sulfuric acid solution dropwise to the reactor to adjust the final pH of the mother liquor to 6.5. After stirring for 1 h, it was filtered to obtain 6.4 g of dry crystalline solid. Dried product uses X-ray powder diffraction, DSC collection of illustrative plates ( figure 2 The solid line in the middle) and the TGA pattern were identified as pseudopolymorph I. The melting point of this pseudopolymorph I was measured to be 114°C-133°C.

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Abstract

The invention discloses an etimicin sulfate pseudo-polymorph, and a preparation method and an application thereof. The X-ray powder diffraction pattern of the pseudo-polymorph has characteristic peaks appearing at 2theta having degrees of 5.1+ / -0.2, 6.0+ / -0.2, 7.0+ / -0.2, 7.6+ / -0.2, 8.5+ / -0.2, 10.9+ / -0.2, 12.5+ / -0.2, 13.1+ / -0.2, 13.7+ / -0.2, 15.5+ / -0.2, 16.0+ / -0.2, 16.6+ / -0.2, 17.2+ / -0.2, 17.6+ / -0.2, 19.4+ / -0.2, 19.9+ / -0.2, 20.1+ / -0.2, 20.5+ / -0.2, 21.7+ / -0.2, 22.6+ / -0.2, 23.2+ / -0.2, 24.0+ / -0.2, 24.5+ / -0.2, 26.0+ / -0.2, 26.7+ / -0.2, 27.1+ / -0.2, 27.6+ / -0.2, 28.4+ / -0.2 and 28.8+ / -0.2. The invention also discloses the preparation method of the pseudo-polymorph, and the application of the pseudo-polymorph in the preparation of medicines for treating human bacterial infectious diseases.

Description

technical field [0001] The present invention relates to novel 1-N-ethyl gentamicin C 1a Pseudopolymorph I of sulfate (etimicin sulfate), its preparation method and its application in the preparation of medicines for treating human bacterial infectious diseases. Background technique [0002] Compound 1-N-ethyl gentamicin C of the following formula (1) 1a Sulfate (commonly known as etimicin sulfate, formerly known as atamycin, antibiotic 89-07) is suitable for the treatment of human bacterial infectious diseases, such as gastrointestinal infection or skin infection. [0003] [0004] Etimicin sulfate is a new generation of semi-synthetic aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria, which is developed by Chinese researchers. [0005] In CN1100467A, Zhao Min, the inventor of etimicin sulfate, etc. reported the chemical structure, preparation method, pharmaceutical dosage form and pharmacological research results of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/236C07H1/06A61K31/7036A61P31/04
Inventor 李继安封成军陈舟舟陈代杰李兴刚蓝鸿
Owner SHANGHAI INST OF PHARMA IND
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