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Method for preparing darunavir amorphous

A technology for darunavir and amorphous substances, which is applied in the field of preparing darunavir amorphous substances, can solve the problems of high temperature, high cost, easy generation of impurities, etc., and achieves simple preparation method, low production cost, and high stability. Good results

Active Publication Date: 2016-04-27
SHANGHAI DESANO PHARMA INVESTMENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The temperature of the fourth and fifth methods above is too high, the operation is inconvenient, the cost is high, and impurities are likely to be generated during the crystallization process, which is not conducive to industrial production

Method used

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  • Method for preparing darunavir amorphous
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  • Method for preparing darunavir amorphous

Examples

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preparation example Construction

[0054] Preparation method of amorphous darunavir

[0055] The invention provides a preparation method of amorphous darunavir, comprising the steps of:

[0056] (1) dissolving darunavir or its solvate in the first solvent described in the present invention to form a first solution containing darunavir;

[0057] Wherein, the solvate may include: darunavir ethanolate, hydrate, methanolate, acetonate, methylene chloride, ethyl acetate, 1-methoxy-2 - propanolate, anisole, tetrahydrofuryl, isopropanolate, mesylate, etc.; preferably methanolate, ethanolate, hydrate, or combinations thereof.

[0058] In another preferred example, the ratio (g / mL) of the mass (W) of darunavir or its solvate to the volume (V) of the first solvent (g / mL) is 1:2-50, preferably 1:5 -15.

[0059] In another preferred example, the dissolution is completed at a temperature of 20-50°C, preferably 25-40°C.

[0060] (2) Mix the first solution containing darunavir with the second solvent of the present invent...

Embodiment 1

[0077] Example 1 Preparation of amorphous darunavir

[0078] At 35°C, dissolve 10g of darunavir ethanolate in 20mL of methanol, and add the resulting solution dropwise into 300mL of cold water (water temperature is 0-5°C) under stirring, and stir for 1-3 hours after the drop is complete . Filtration, the filter cake was washed with about 50mL of water, and dried to obtain 9.5g of white solid, which was detected as amorphous darunavir, and its XRPD pattern was as follows: figure 1 As shown, the IR diagram is as figure 2 As shown, the DSC diagram is shown in image 3 shown.

Embodiment 2

[0079] Example 2 Preparation of amorphous darunavir

[0080] At room temperature, dissolve 200g of darunavir methanolate in a mixed solvent containing 1000ml of methanol and 1000ml of ethanol, and add the resulting solution dropwise to 4L of cold water (water temperature is 5-10°C) under stirring. Stir for 1-2 hours. After filtering, the filter cake was washed with about 200 mL of water and dried to obtain 192 g of white solid. After testing, it is amorphous darunavir, and its XRPD pattern, FTIR pattern, and DSC pattern are basically consistent with those in Example 1.

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Abstract

The invention relates to a preparation method of a Darunavir amorphous matter. Specifically, the method disclosed by the invention comprises the steps of: mixing a Darunavir-containing first solution with a second solvent so as to obtain precipitated amorphous Darunavir. The product made by the method has high purity and good stability. The method has the advantages of simple operation, low production cost, environmental friendliness, and suitability for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a method for preparing darunavir amorphous. Background technique [0002] Darunavir, whose trade name is Prezista, is a first-generation non-peptide HIV protease inhibitor developed by Tibotec, a subsidiary of Johnson & Johnson. Its structural formula is shown in the following formula. [0003] [0004] Darunavir selectively inhibits the HIV-encoded Gag-Pol polyprotein in infected cells, preventing the formation of mature virions. Both in vivo and in vitro experiments have proved that darunavir still has strong antiviral activity against HIV that has developed drug resistance, and the tendency of the virus to develop drug resistance to darunavir is low. [0005] In the prior art, WO03 / 106461 has reported various polymorphic forms of darunavir and preparation methods thereof: A-type crystallization (ethanol solvate), B-type crystallization (hydrate), C-type cryst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 李金亮赵楠王锰
Owner SHANGHAI DESANO PHARMA INVESTMENT
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