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Preparation method of azacitidine single crystal

Azacitidine single crystal and azacitidine technology, applied in the field of preparation of azacitidine single crystal

Active Publication Date: 2018-03-23
北京满格医药科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Single crystal of azacitidine has no public reports

Method used

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  • Preparation method of azacitidine single crystal
  • Preparation method of azacitidine single crystal
  • Preparation method of azacitidine single crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1 Azacitidine is refined, and the process is as follows:

[0058] Under nitrogen protection, add 130 mL of dimethyl sulfoxide (DMSO) into a four-neck flask, raise the temperature to 70-75°C, slowly add 50 g of crude azacitidine, and stir until it dissolves. Add 1.5g of activated carbon, control the temperature at 70°C, and stir for 30 minutes to decolorize. Precision filtration. Add 0.1g of sodium methoxide solid to the obtained liquid, add 35mL of methanol dropwise, stir at 55-60°C for 2 hours, add 550mL of methanol dropwise, cool down to room temperature after dropping, filter, and wash with 100mL of methanol to obtain 43g of wet product. ℃, -0.09MPa vacuum drying to constant weight under reduced pressure to obtain 40.4g of azacitidine. HPLC purity 99.84%.

Embodiment 2

[0059] Embodiment 2 single crystal cultivation process

[0060] Add 0.5 g of the solid azacitidine obtained in Example 1 to a 25 mL beaker, then add 1 mL of dimethyl sulfoxide (DMSO), and gently stir with a glass rod to dissolve. Then add 0.5mL of methanol and 1mL of toluene, and continue stirring with a glass rod until clear. Then filter it with a 0.25μm membrane filter into another clean 25mL beaker. Seal the beaker with parafilm or plastic wrap, and then use a needle to pierce 10 small holes on the parafilm (as far as possible to ensure that the pricked small holes are evenly distributed). This beaker is numbered A. Take another 100mL beaker, numbered B. Add 20mL of dichloromethane to it, then put beaker A into beaker B, and seal beaker B with parafilm. Then place it in an environment with a constant temperature of 25°C and a humidity of 50%, avoid shaking, and let it stand for about one to two weeks. Observe every 2 hours on the first day, if no crystals appear, obser...

Embodiment 3

[0061] Example 3 In this example, on the basis of Example 2, a saturated solution is directly prepared, and the single crystal formation time is significantly shorter than that in Example 2. The process is as follows:

[0062] Add 0.5 g of the solid azacitidine obtained in Example 1 to a 25 mL beaker, then add 1 mL of dimethyl sulfoxide (DMSO), and gently stir with a glass rod to dissolve. Then add 0.2mL of methanol and 1mL of toluene, and continue stirring with a glass rod until clear. At this time, use a dropper to add dichloromethane dropwise to the clear solution. During the dropping process, some parts will become turbid. At this time, wait until the turbidity disappears and continue to drop until the system becomes slightly turbid. When the system does not disappear after shaking, stop the dropwise addition. dichloromethane. At this point a saturated solution of azacitidine is considered to be obtained. Then use a 0.25μm filter membrane to filter into another clean 25m...

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Abstract

The invention belongs to the technical field of the preparation of bulk drugs, and particularly relates to a preparation method of an azacitidine single crystal. According to the technical scheme of the preparation method, the preparation method comprises the following steps of firstly taking a certain amount of azacitidine solid, adding a proper amount of organic solvent (one or more mixed solvents) at some temperature, dissolving, then filtering through a microporous filtering film, so as to obtain an azacitidine solution with a certain concentration, and meanwhile, guaranteeing the obtainedsolution to be clear and transparent and to have no any macroscopic particles; afterwards, culturing the azacitidine single crystal by adopting a volatile solvent diffusion method. The invention provides a culture method of the azacitidine single crystal, and a scientific method is provided for the quality control of an azacitidine bulk drug, particularly for the confirmation of an absolute configuration of a chiral center.

Description

technical field [0001] The invention belongs to the technical field of raw material medicine preparation, and in particular relates to a preparation method of azacitidine single crystal. Background technique [0002] Azacitidine (azacitidine), the chemical name is 1-(β-D-ribofuranosyl)-4-amino-1,3,5-triazin-2(1H)-one, also known as 5-azacytidine Glycoside, azacytidine, its structure is as follows: [0003] [0004] Azacitidine is a white needle-like crystal. It is a DNA methyltransferase inhibitor developed by Pharmion Company of the United States. It was first launched in the United States in July 2004. It is a cell cycle-specific drug that acts on the S phase and can be rapidly phosphorylated. And penetrate into RNA (ribonucleic acid) and DNA (deoxyribonucleic acid) by destroying the smooth translation of nucleic acid into protein, inhibiting the synthesis of protein, and can also affect the synthesis of pyrimidine by inhibiting orotate nucleotide decarboxylase; clinic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/12C07H1/06
CPCC07B2200/13C07H1/06C07H19/12
Inventor 赵乾坤彭涛卢作勇汪娟
Owner 北京满格医药科技有限公司
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