Idelalisib amorphous substance and preparation method thereof

A technology of amorphous substances and solvents, which is applied in the field of amorphous substances of Idelib and its preparation, can solve the problems of inconvenient development of pharmaceutical solid preparations with water content of amorphous substances, difficult to remove water, high solubility, etc., and achieves good performance. Effects of physical and chemical stability, reduction of solvent residues, and simple preparation method

Inactive Publication Date: 2017-05-24
宁波爱诺医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dichloromethane has greater solubility to Adlib, and using dichloromethane as an anti-solvent will greatly affect the yield; water is used as an anti-solvent, and the water attached to the amorphous is difficult to remove, and the water content of the amorphous is too high. The General Assembly brings inconvenience to the development of pharmaceutical solid dosage forms

Method used

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  • Idelalisib amorphous substance and preparation method thereof
  • Idelalisib amorphous substance and preparation method thereof
  • Idelalisib amorphous substance and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Adlib (1 g) was added to tetrahydrofuran (5 ml), and stirred at 50°C to dissolve. The above solution was added to a mixed solvent (35 ml) of methanol and water (1:10, weight ratio) cooled to -15°C, a white solid was precipitated under stirring, filtered, and vacuum-dried at 40-50°C to obtain a solid 0.92 Gram, solvent residue: tetrahydrofuran 521ppm, methanol 1321ppm, X-ray powder diffraction pattern as figure 1 shown.

Embodiment 2

[0043] Adlib (1 g) was added to acetonitrile (10 ml), stirred and dissolved at room temperature. The above solution was added to a mixed solvent (60 ml) of ethanol and water (1:10, weight ratio) cooled to 10°C, a white solid was precipitated under stirring, filtered, and vacuum-dried at 40-50°C to obtain 0.93 g of a solid , Solvent residue: acetonitrile 320ppm, ethanol 983ppm.

Embodiment 3

[0045]Add Adlib (1 g) to acetone (10 ml), stir and dissolve at room temperature. The above solution was added to a mixed solvent (100 ml) of tetrahydrofuran and water (1:20, weight ratio) cooled to 10°C, a white solid was precipitated under stirring, filtered, and vacuum-dried at 40-50°C to obtain 0.91 g of a solid , Solvent residue: acetone 780ppm, tetrahydrofuran 230ppm.

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Abstract

The invention relates to a preparation method of an Idelalisib amorphous substance. The Idelalisib amorphous substance prepared by the method can effectively reduce solvent residue; and through a conventional vacuum drying means, the amorphous substance of which the solvent residue conforms to the specifications of ICH (International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use) can be obtained. The amorphous substance can keep favorable physical stability and chemical stability under accelerated test conditions (the temperature is 40+/-2 DEG C, and the humidity is 75%+/-5%).The preparation method of the Idelalisib amorphous substance is simple to operate and easy to realize industrial production.

Description

technical field [0001] The invention relates to an amorphous substance of Adlib and a preparation method thereof. Background technique [0002] Idelalisib, the chemical name is 5-fluoro-3-phenyl-2-[(1S)-1-(9H-purin-6-ylamino)propyl]-4(3H)-quinazole Phenone, its structure is shown in formula (I): [0003] [0004] Adlib (trade name Zydelig) is a selective phosphoinositide 3-kinase delta (PI3K-delta, P110-delta) inhibitor developed by Gilead Science. On July 23, 2014, the U.S. Food and Drug Administration (FDA) approved three indications of Adlib: in combination with rituximab (Rituxan) for the treatment of relapsed chronic lymphocytic leukemia (CLL), as a monotherapy Drug therapy for relapsed follicular B-cell non-Hodgkin's lymphoma (FL) and relapsed small lymphocytic lymphoma (SLL). The FDA has accelerated approval for the latter two indications, and the patients have received at least two previous systemic treatments. [0005] Adlib is the first marketed oral, select...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/34
CPCC07D473/34C07B2200/13
Inventor 张席妮周涛胡涛熊志刚
Owner 宁波爱诺医药科技有限公司
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