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A new crystal form of romidepsin and its preparation method and application

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

Active Publication Date: 2018-01-09
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 CN201210579007.4 has a product purity greater than 99% and a total yield greater than 30%

Method used

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  • A new crystal form of romidepsin and its preparation method and application
  • A new crystal form of romidepsin and its preparation method and application
  • A new crystal form of romidepsin and its preparation method and application

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 chloroform:methanol=9 / 1 (volume ratio) mixed solvent to form a saturated solution (some crystals were not completely dissolved), and the filtrate was obtained by filtration. Take 3ml of the filtrate, then add 27ml of acetonitrile to the filtrate, mix well and place in a refrigerator at 4°C in the dark, after 72h, filter to obtain crystals, and dry the crystals in vacuum at 45°C for 48h to obtain romidepsin crystal form O. Get sample detection, its X-ray powder diffraction pattern is as follows figure 1 As shown, the infrared absorption spectrum is shown as figure 2 As shown, the DSC spectrum is as image 3 As shown, the TGA spectrum is as Figure 4 shown.

Embodiment 2

[0047] 10.0 g of romidepsin (HPLC purity greater than 99%) was dissolved in 25 ml of chloroform:methanol=9 / 1 (volume ratio) mixed solvent to form a saturated solution (with crystals not completely dissolved), and filtered to obtain the filtrate. Take 11 parts of 1ml filtrate, then add 1ml, 2ml, 3ml, 4ml, 5ml, 6ml, 7ml, 8ml, 9ml of acetonitrile to the filtrate respectively, mix well and place in a refrigerator at 4°C in the dark, and filter to obtain crystals after 48 hours , the crystals were vacuum-dried at 45°C for 48 hours. After testing, the crystal forms obtained in 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 methylene chloride: in the mixed solvent of ethanol=9 / 1 (volume ratio), then added 35ml acetonitrile, stirred overnight at room temperature, filtered, 45 ℃ vacuum After drying for 48 hours, 0.92 g of solid was obtained with a yield of 92%. After detection, it was confirmed that romidepsin crystal form O was obtained.

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Abstract

The present invention relates to a novel polymorph form O of romidepsin. Said polymorph can be expressed by an X-ray powder diffraction (XRPD) spectrogram, a differential scanning calorimetry (DSC) spectrogram, and an infrared (IR) absorption spectrogram. At the same time, the present invention also relates to a pharmaceutical composition of the remidepsin polymorph form O, a preparation method for same, and uses thereof.

Description

technical field [0001] The present invention relates to the field of pharmacy. 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 treating malignant tumors is the primary task of drug researchers. Among the anti-tumor drugs, the research and development of non-cytotoxic drugs that selectively inhibit the growth of cancer cells is the current research focus of anti-tumor drugs. In recent years, a class of zinc ion-dependent metalloproteinases—histone deacetylases (HDACs) has become a hot spot in the research of anticancer drugs. [0003] Romidepsin, also known as FK228 and FR901228, is an HDAC inhibitor. HDACs catalyze the removal of acetyl groups from ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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