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Preparation method of amorphous dasatinib

A dasatinib and amorphous technology, which is applied in the field of producing amorphous dasatinib, can solve problems such as numerous operation steps, loss of dasatinib, complex refining methods, etc., and achieves low process pollution, complete dissolution, and easy operation The effect of fewer steps

Active Publication Date: 2015-02-04
深圳市新浩瑞医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the refining method is complicated, the operation steps are numerous, and a variety of solvents are used, it is easy to cause the loss of dasatinib

Method used

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  • Preparation method of amorphous dasatinib
  • Preparation method of amorphous dasatinib
  • Preparation method of amorphous dasatinib

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preparation example Construction

[0034] The invention provides a preparation method of amorphous dasatinib, which firstly dissolves the raw materials of various crystal forms of dasatinib with anhydrous solvent and co-solvent, and then uses spray drying and cyclone separation methods to rapidly precipitate dasatinib The solid powder of tinib is then dried under reduced pressure to remove the solvent to obtain the dasatinib amorphous product whose residual solvent complies with the Chinese Pharmacopoeia. The method of the present invention is described in detail below:

[0035] (1) Dissolution of various crystal forms of dasatinib

[0036] Add the raw materials of various crystal forms of dasatinib into a certain amount of solvent, and add a certain amount of co-solvent, stir and heat to 60-100°C to dissolve until the raw materials of dasatinib are completely dissolved. The solvent should be an anhydrous organic solvent that is soluble in dasatinib, such as ethanol, isopropanol, acetone, etc. The mass ratio ...

Embodiment 1

[0048] Add 10 g of dasatinib raw material to 100 g of ethanol, and add 0.1 g of DMF as a cosolvent. Heat at 80°C to dissolve, enter Buqi B-290 spray dryer while it is hot, control hot air heating temperature at 100-150°C, hot air outlet temperature at 80-100°C, control vacuum degree to less than -0.095MPa, flow control and cyclone separation and collection It is suitable for solid powder. After spray-drying, the collected solid powder enters a decompression oven, heats and dries at 80°C for 6 hours under high vacuum, further dries, and removes the solvent to obtain Dasatinib amorphous solid with a yield of 99.2%, purity and addition The Dasatinib raw material is relatively unchanged, and the X-ray diffraction pattern of the powder is as follows: figure 1 shown. from figure 1 Looking at it, no sharp diffraction angle peaks were found, proving that the product is amorphous dasatinib. After the Karl Fischer moisture test, the moisture content is less than 2%. As determined b...

Embodiment 2

[0053] 10 g of dasatinib raw material was added to 150 g of isopropanol, and 0.1 g of DMSO was added as a cosolvent. Heat at 80°C to dissolve, enter Buqi B-290 spray dryer while it is hot, control hot air heating temperature at 100-150°C, hot air outlet temperature at 80-100°C, control vacuum degree to less than -0.095MPa, flow control and cyclone separation and collection It is suitable for solid powder. After spray-drying, the collected solid powder enters a decompression oven, heats and dries at 80°C for 8 hours under high vacuum, further dries, and removes the solvent to obtain Dasatinib amorphous solid with a yield of 99.6%, purity and addition The raw material dasatinib was relatively unchanged. From the X-ray diffraction pattern, combined with the DSC and TGA patterns, it can be known that the prepared dasatinib is amorphous dasatinib. After the Karl Fischer moisture test, the moisture content is less than 2%. As determined by headspace gas chromatography, the residu...

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Abstract

The invention relates to a preparation method of amorphous dasatinib, wherein the preparation method includes the steps: dissolving raw materials of various crystal types of dasatinib in an anhydrous organic solvent at the temperature of 60-100 DEG C, adding a cosolvent for helping dissolution, and thus obtaining a fully-dissolved dasatinib solution; carrying out spray drying on the dasatinib solution, carrying out cyclone isolation, and rapidly precipitating to obtain a dasatinib solid powder; drying the dasatinib solid powder under reduced pressure, removing the solvent, and thus obtaining the dasatinib amorphous product. Through testing, the prepared amorphous dasatinib has the moisture content generally less than 2%, and is nearly anhydrous dasatinib. The method is suitable for converting various crystal types of dasatinib into the dasatinib amorphous product having the residual solvent consistent with Chinese pharmacopoeia, and the preparation yield reaches up to more than 99%. Moreover, the method has the advantages of simple operation, less operation steps, less using solvent, small process pollution, low cost and the like, and is suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to a method for producing amorphous dasatinib, which belongs to the technical field of pharmacy. Background technique [0002] Dasatinib (BMS-354825, Dasatinib) is a tyrosine kinase inhibitor for the treatment of chronic myelogenous leukemia (Chronic Myelogenous Leukemia, CML) and Philadelphia chromosome in the late stage of imatinib treatment. Positive acute myeloid leukemia, the drug has also been proven to treat many other types of cancer, such as accelerated prostate cancer. [0003] The preparation methods of dasatinib disclosed in the current literature mainly focus on the synthesis of various crystal forms of dasatinib, but there is little disclosure on how to prepare amorphous dasatinib. For example, the authorized CN 1980909 protects dasatinib with a crystal water, that is, its monohydrate crystal form, and discloses the preparation method of the monohydrate crystal form, but does not mention amorphous dasatinib Ni's pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12
CPCC07D417/12
Inventor 金鹏
Owner 深圳市新浩瑞医药科技有限公司
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