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Idelalisib crystal form C and preparation method thereof

A technology of Idelalis and its crystal form, which is applied in the field of medicinal chemistry and can solve problems such as poor solubility, large static electricity, and crystal form A with large static electricity.

Inactive Publication Date: 2018-06-29
JIANGSU CHUANGUO PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] WO2005113556 discloses Idelaris and its preparation method, and later research shows that: using the preparation method, the solvate of Idelalis containing 0.4 molecules of ethanol (referred to as crystal form I in WO2015014315 international patent application) is obtained , WO2015014315 stated that it has the following defects: the weight change is about 0.95% in the range of 20-80% relative humidity, it has certain hygroscopicity, and its stability is poor
Although the crystal form A has better thermal stability, high humidity stability and pressure stability, but the crystal form A has relatively high static electricity and is easy to coalesce during the preparation process
[0012] To sum up, there are many crystal forms of Aderaris, but the crystal forms may have poor stability, poor solubility, high static electricity, or unsuitable for industrial production. Therefore, it is necessary to find a crystal form that is both A crystal form with good solubility and stability and low electrostatic interaction, which is suitable for the industrial preparation of preparations and meets various performance requirements of preparations

Method used

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  • Idelalisib crystal form C and preparation method thereof
  • Idelalisib crystal form C and preparation method thereof
  • Idelalisib crystal form C and preparation method thereof

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preparation example Construction

[0100] In a preferred embodiment of the present invention, the preparation method comprises the following steps:

[0101] a) Dissolving the ederalix raw material in an organic solvent, the dissolving temperature is 15-120°C (preferably 20°C-80°C) to obtain a clear solution;

[0102] b) Concentrate the above solution at 20-40°C until a small amount of turbidity occurs;

[0103] c) at 0~60°C (preferably 0~50°C), dropwise add anti-solvent water to the solution obtained in step a) for crystallization;

[0104] d) heat preservation and stirring;

[0105] e) cooling to room temperature, filtering and drying to obtain the idelalix crystal form C.

[0106] The crystal form of the idelalix raw material is not limited, and it can be amorphous or any known crystal form or a mixture thereof.

[0107] Said solvent refers to the solvent that can completely dissolve the raw material of ederalix in it at 15~120℃, including but not limited to methanol, ethanol, acetone, acetonitrile, tetrah...

Embodiment 1

[0130] Example 1: Preparation of idelalix crystal form C

Embodiment 11

[0132] At 40°C, 1 g of ederalix raw material (crystal form I referred to in the WO2015014315 international patent application) was dissolved in 30 mL of tetrahydrofuran to obtain a clear solution; the solution was concentrated at 25°C until turbidity appeared; At 40°C, anti-solvent water was slowly added dropwise to the above solution, and after the solid was precipitated, the crystallization was carried out for 2 hours under heat preservation and stirring, and then cooled to room temperature; filtered and dried to obtain 0.90 g of crystal; the yield was 90%, and the HPLC purity was 99.2% .

[0133] figure 1 is the XRD pattern of the obtained crystal, from figure 1 Visible: under powder X-ray diffraction, the crystal has 2θ at 9.8±0.2°, 11.7±0.2°, 12.7±0.2°, 15.3±0.2°, 18.3±0.2°, 19.0±0.2°, 23.1±0.2°, 25.6± There is a characteristic peak at 0.2°.

[0134] Further, under the powder X-ray diffraction, the crystal form C of idelalix of the present invention has 2θ of 9.8±0.2°,...

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Abstract

The invention relates to an idelalisib crystal form C and a preparation method thereof. Particularly, the idelalisib crystal form C has the advantages that the purity is high; compared with 4-moleculehydrate and 0.7-molucule hydrate, the heat stability is better, and the wet stability and pressure stability are higher; the electrostatic function is small; the idelalisib crystal form C is suitablefor the industrialized preparation of preparations, and meets the property requirements of the preparations; the preparation technology is simple, the operability is strong, the technology conditionsare mild, the yield rate is high, the quality is stable, the cost is low, the production cycle is short, and the scale production can be easily realized.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a crystal form C of idelalix and a preparation method thereof. Background technique [0002] Idelalis, English name Idelalisib, its chemical name: (S)-2-(1-(9H-purin-6-ylamino)propyl)-5-fluoro-3-phenylquinazoline- 4(3H)-ketone, trade name: Zydelig, molecular formula: C 22 H 18 FN 7 O, molecular weight: 415.42, CAS number: 870281-82-6, chemical structural formula: [0003] [0004] The drug is a phosphatidylinositol 3-kinase delta inhibitor (referred to as PI3Kdelta inhibitor) developed by Gilead, which is used for chronic lymphocytic leukemia, indolent non-Hodgkin's lymphoma, mantle cell lymphoma, diffuse large The treatment of B-cell lymphoma, Hodgkin's lymphoma, multiple myeloma, acute myeloid leukemia and hematological malignancies was approved by the FDA on July 23, 2014. [0005] WO2005113556 discloses idelalix and its preparation method. Later studies show that: u...

Claims

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Application Information

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IPC IPC(8): C07D473/34A61K31/52A61P35/00A61P35/02
CPCC07D473/34C07B2200/13
Inventor 申淑匣修平张良
Owner JIANGSU CHUANGUO PHARMA CO LTD
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