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Fidaxomycin crystal form II and preparation method thereof

A technology of fidaxomicin and crystal form, which is applied in the field of fidaxomicin crystal form II and its preparation, can solve the problems of poor crystal form stability and shorten product shelf life, achieve low cost, avoid environmental pollution and human body damage and good stability

Active Publication Date: 2016-07-06
NCPC NEW DRUG RES & DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After research, it was found that the stability of the crystal form was poor, and after being placed at 40°C for 30 days, there was a degradation peak detected by liquid chromatography, which shortened the shelf life of the product

Method used

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  • Fidaxomycin crystal form II and preparation method thereof
  • Fidaxomycin crystal form II and preparation method thereof
  • Fidaxomycin crystal form II and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take 1.5 g of fidaxomicin, add 70 ml of a mixed solvent prepared by ethyl acetate:methylcyclohexane with a volume ratio of 1:1, and sonicate at room temperature for 1 minute to obtain a supersaturated solution. Crystallized at room temperature for 7 days. Suction filtration under reduced pressure, and the filter cake was vacuum-dried in an oven at 40°C for 2 hours to obtain Fidaxomycin Form II.

[0047] Measure the XRD value of the made Fidaxomycin crystal form II as shown in Table 1, and the spectrum is as follows figure 1 As shown, the figure shows that there are X-ray powder diffraction peaks in the X-ray powder diffraction pattern at 7.04°, 15.87°, 19.14°, 20.46° and 22.95±0.2°2θ.

[0048] The TGA and DSC spectra of Fidaxomycin crystal form II are measured as figure 2 shown.

[0049] The 1H-NMR spectrum of Fidaxomycin crystal form II is measured as image 3 shown.

Embodiment 2

[0051] Take 1.5 g of fidaxomicin, add 70 ml of a mixed solvent prepared by heptane:ethyl acetate at a volume ratio of 1:1, and ultrasonicate at room temperature for 3 minutes to obtain a supersaturated solution. Placed at 40°C for 10 days to crystallize. Suction filtration under reduced pressure, and the filter cake was vacuum-dried in an oven at 20°C for 6 hours to obtain Fidaxomycin Form II.

Embodiment 3

[0053] Take 1.5 g of fidaxomicin, add 150 ml of a mixed solvent prepared by ethyl acetate:methylcyclohexane at a ratio of 0.1:1, and sonicate at room temperature for 5 minutes to obtain a supersaturated solution. Crystallize at 10°C for 5 days. Suction filtration under reduced pressure, and the filter cake was vacuum-dried in an oven at 30°C for 4 hours to obtain crystalline form II of Fidaxomycin.

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Abstract

The invention discloses a fidaxomicin crystal form II and a preparation method thereof. An X-ray powder diffraction spectrum of the crystal formula has X-ray powder diffraction peaks at 2theta, namely 7.04 degrees, 15.87 degrees, 19.14 degrees, 20.46 degrees and 22.95 + / -0.2 degrees. The crystal form obtained by the method is stable, simple in preparation method, strong in maneuverability and applicable to industrial production.

Description

technical field [0001] The present invention relates to a crystal form of a compound and a crystallization method thereof, more precisely, to fidaxomicin crystal form II and a preparation method thereof. Background technique [0002] Fidaxomicin is a new macrolide antibiotic with an 18-membered ring structure produced by the fermentation of D. aurantiacus. It is mainly resistant to Gram-positive aerobic and anaerobic bacteria, Clostridium difficile, and also has good antibacterial effect on methicillin-resistant Staphylococcus aureus, Clostridium perfringens and Enterococcus. Fidaxomicin is mainly used clinically for the treatment of diseases caused by Clostridium difficile infection. It has the advantages of low tendency to develop resistance, long-lasting post-antibiotic effect, low cross-resistance and few adverse reactions. [0003] [0004] Fidaxomicin is a polymorphic compound, usually in the form of white needles, snowflake crystals or amorphous powder. Due to th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06A61K31/7048A61P31/04
Inventor 张雪霞任风芝段宝玲陈书红李晓露佟杰王海燕李宁李丽红胡卫国
Owner NCPC NEW DRUG RES & DEV
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