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A kind of doripenem hydrate crystal and preparation method thereof

A technology of doripenem and hydrate, which is applied in the field of doripenem hydrate crystals and its preparation, can solve the problems that the crystal form IV cannot be directly obtained, the preparation process is complicated, and the preparation cost is high, so as to achieve good stability and high production cost. Simple, pure effect

Active Publication Date: 2011-12-21
SHANGHAI ACEBRIGHT PHARMA CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Among the above four crystal forms, the stability of the three crystal forms I, II, and III is not good, and only the crystal form IV is the most stable crystal form among them. However, the crystal form IV cannot be directly obtained, and the crystal form must be obtained first. After type III, it is obtained by drying under reduced pressure, which undoubtedly has defects such as complicated preparation process and high preparation cost.

Method used

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  • A kind of doripenem hydrate crystal and preparation method thereof
  • A kind of doripenem hydrate crystal and preparation method thereof
  • A kind of doripenem hydrate crystal and preparation method thereof

Examples

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Effect test

Embodiment 1

[0052] Dissolve 5g of crude doripenem in 100mL of distilled water at 50-55°C, then cool down to 25°C in a water bath, add 0.5g of activated carbon, stir for 15 minutes to decolorize; Precipitation, stirring for two hours, suction filtration, washing the filter cake with isopropanol / water = 4:1; drying at 50-60° C., 5 mmHg for 1.5 hours, to obtain 2 g of doripenem hydrate crystals of the present invention.

[0053] Refer to the method described in "Journal of Chromatography B, 853 (2007), 123-126" to detect the HPLC purity of the obtained crystals; Residual amount of isopropanol in the crystals.

[0054] It is found through detection that the HPLC purity of the crystals obtained in this example is 99.85%, and the residual amount of isopropanol is 219ppm.

[0055] The water content in the crystal was determined to be 4.83% by Karl Fischer (KF) method.

[0056] The powder X-ray diffraction spectrogram of the crystal obtained in the present embodiment is as follows figure 1 Sho...

Embodiment 2

[0061] Dissolve 10g of crude doripenem in 200mL of distilled water at 50-55°C, then cool down to 25°C in a water bath, add 1.0g of activated carbon, stir for 15 minutes to decolorize; filter with suction, cool the filtrate to about 0-10°C, and add The 0.1g crystal obtained in Example 1 is used as a seed crystal, and solids are precipitated. After stirring for 1 hour, 100ml of isopropanol is added dropwise, and after the dripping is completed and stirred for 2 hours, suction filtration is performed, and the filter cake is washed with isopropanol / water=4:1; Dry at 50-60°C and 10mmHg for 2 hours to obtain 8.2g of crystals.

[0062] It is detected that: the HPLC purity of the crystal obtained in this embodiment is 99.86%, the residual amount of isopropanol in it is 205ppm, and the moisture measured by the Karl-Fischer (KF) method is 4.79%; and has figure 1 The powder X-ray diffraction spectrum shown, figure 2 The DSC spectrum shown, image 3 The TG spectrum shown and Figure 4...

Embodiment 3

[0064] Dissolve 10 g of crude doripenem in 110 mL of distilled water at 55-60 °C, then cool down to 15 °C in a water bath, add 1.0 g of activated carbon, stir for 15 minutes to decolorize; filter with suction, and add 0.1 g of the crystal obtained in Example 1 as a seed crystal , there is solid precipitation, after stirring for 1 hour, add 200ml of isopropanol dropwise, and cool to 0-5°C after dropping, after stirring for 2 hours, filter with suction, wash the filter cake with isopropanol / water=4:1, at 50-60 ℃, 10mmHg and dried for 1.5 hours to obtain 8.0g of crystals.

[0065] It is detected that: the HPLC purity of the crystal obtained in this embodiment is 99.83%, the residual amount of isopropanol in it is 259ppm, and the moisture measured by the Karl-Fischer (KF) method is 4.81%; and has figure 1 The powder X-ray diffraction spectrum shown, figure 2 The DSC spectrum shown, image 3 The TG spectrum shown and Figure 4 Infrared (IR) spectral features shown.

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Abstract

Disclosed are a doripenem hydrate crystal and preparation method therefor. The X-ray diffraction spectrogram of the crystal powder is basically as represented in figure 1, and the measured water content is 4.4 to 5.5%. The doripenem hydrate crystal of the present invention has high purity, low residual solvent, good stability, and application safety. Additionally, the preparation method for the doripenem hydrate crystal of the present invention has simple techniques and low preparation cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a doripenem hydrate crystal and a preparation method thereof, belonging to the technical field of organic chemistry. Background technique [0002] Doripenem (Doripenem) is a new type of β-methyl carbapenem antibiotic developed by Shionogi Pharmaceutical Co., Ltd. in Japan. It was launched in Japan on September 16, 2005, and its trade name is Finibax. Doripenem was approved by the US FDA on October 15, 2007 for the clinical treatment of complicated intra-abdominal infections and complicated urinary tract infections. By inhibiting cell wall synthesis, it shows broad-spectrum and high-efficiency antibacterial activity, especially the activity against Pseudomonas aeruginosa is stronger than the existing carbapenem antibiotics. Its chemical structural formula is as follows: [0003] [0004] Chinese patents (Patent Nos. ZL92111069.3 and ZL95104834.1) disclose the preparation method of amorphous doripenem. As we all know, amorph...

Claims

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Application Information

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IPC IPC(8): C07D477/20C07D477/02
CPCC07D477/02A61K31/407C07D477/20A61P31/04
Inventor 安晓霞吕锋胡猛周吴王光华
Owner SHANGHAI ACEBRIGHT PHARMA CO LTD
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