New crystal form of romidepsin, and preparation method and application thereof

A kind of technology of romidepsin and crystal form, applied in the field of pharmacy

Active Publication Date: 2015-01-07
ZHEJIANG HISUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of romidepsin disclosed in patent CN20121057900...

Method used

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  • New crystal form of romidepsin, and preparation method and application thereof
  • New crystal form of romidepsin, and preparation method and application thereof
  • New crystal form of romidepsin, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 2.0 g romidepsin (HPLC purity greater than 99%) was dissolved in 5 ml of a mixed solvent of chloroform:methanol = 9 / 1 (volume ratio) to form a saturated solution (crystals were not completely dissolved), and the filtrate was obtained by filtration. Take 3ml of the filtrate, and then add 27ml of acetonitrile to the filtrate, mix well and place in a refrigerator at 4°C to avoid light. After 72h, the crystal is filtered and dried at 45°C under vacuum for 48h to obtain romidepsin crystal form O. Take a sample for testing, and its X-ray powder diffraction pattern is as follows figure 1 As shown, the infrared absorption spectrum is as figure 2 As shown, the DSC spectrum is as image 3 As shown, the TGA map is as Figure 4 Shown.

Embodiment 2

[0047] 10.0 g of romidepsin (HPLC purity greater than 99%) was dissolved in 25 ml of a mixed solvent of chloroform: methanol = 9 / 1 (volume ratio) to form a saturated solution (crystals were not completely dissolved), and the filtrate was obtained by filtration. Take 11 parts of 1ml filtrate, and then add 1ml, 2ml, 3ml, 4ml, 5ml, 6ml, 7ml, 8ml, 9ml acetonitrile to the filtrate, mix well and place in a refrigerator at 4℃ to avoid light, and filter to obtain crystals after 48h The crystals were dried in vacuum at 45°C for 48 hours. After testing, the crystal forms obtained by each solvent system are shown in the table below.

[0048] Acetonitrile (m1)

Embodiment 3

[0050] 1.0g romidepsin (HPLC purity greater than 99%) was dissolved in 2.5ml dichloromethane: ethanol = 9 / 1 (volume ratio) mixed solvent, then 35ml acetonitrile was added, stirred overnight at room temperature, filtered, and vacuum at 45°C After drying for 48 hours, 0.92 g of solid was obtained with a yield of 92%. After testing, it was confirmed that the crystalline form O of romidepsin was obtained.

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Abstract

The invention relates to a new crystal form O of romidepsin, which can be characterized by X-ray powder diffraction (XRD) spectrogram, differential scanning calorimetry (DSC) spectrogram, infrared absorption (UV) spectrogram and the like. Meanwhile, the invention also relates to a preparation method and application of the romidepsin crystal form O.

Description

Technical field [0001] The invention relates to the field of pharmaceuticals. More specifically, the present invention relates to a new crystal form of romidepsin and the preparation method and application of the new crystal form. technical background [0002] Malignant tumors are one of the most serious diseases threatening human health. For a long time, tumor treatment has been a major research topic in the medical field, and finding new drugs for the treatment of malignant tumors is the primary task of drug researchers. Among anti-tumor drugs, the research and development of non-cytotoxic drugs that selectively inhibit the growth of cancer cells is the current focus of anti-tumor drugs. In recent years, a type of zinc ion-dependent metalloprotease—histone deacetylases (HDACs) has become a hot spot in the research of anti-tumor drugs. [0003] Romidepsin, also known as FK228 and FR901228, is an HDAC inhibitor. HDACs catalyze the removal of acetyl groups from acetylated lysine...

Claims

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Application Information

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IPC IPC(8): C07K5/103C07K1/02A61K38/07A61P35/00
CPCA61K38/07C07K1/02
Inventor 张辉王继栋杜敏娜郑玲辉骆红英白骅
Owner ZHEJIANG HISUN PHARMA CO LTD
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