Crystal form, pharmaceutical composition, preparation method and use of Idelalis

A technology of composition and crystal form, applied in the direction of drug combination, organic chemical method, active ingredient of heterocyclic compound, etc., can solve the problems that the preparation method needs to be continuously improved

Inactive Publication Date: 2018-11-20
HUBEI BIO PHARMA IND TECHCAL INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the crystal form of the drug compound has been studied in the prior art, both the characteristics of its crystal form and its preparation method need to be continuously improved

Method used

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  • Crystal form, pharmaceutical composition, preparation method and use of Idelalis
  • Crystal form, pharmaceutical composition, preparation method and use of Idelalis
  • Crystal form, pharmaceutical composition, preparation method and use of Idelalis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0117] Example 1: Preparation of Idelaris Form R

[0118] In a 3L glass bottle, add 200 g of idelaris as an amorphous solid, add 200 ml of dichloromethane, and 50 ml of absolute ethanol, stir mechanically, and heat to reflux at 40°C. After starting to reflux, 1.6 L of acetonitrile was added dropwise, while continuing to raise the temperature to 55°C. The dropwise addition was completed in 5 minutes, and stirring was continued for 30 minutes. Rapid cooling down to 5°C. A large amount of product was precipitated, and the stirring was continued for 1 hour, and the product was obtained by filtration, and the solid was dried in a blast drying oven at 55° C. for 8 hours to obtain 190 g of Idelalis crystal form R, and its X-ray powder diffraction pattern was as follows: figure 1 shown.

Embodiment 2

[0119] Example 2: Preparation of Idelaris Form R

[0120] In a 3L glass bottle, add 200g of idelaris amorphous solid, add 200ml of dichloromethane, 50ml of absolute ethanol, stir magnetically, and heat to 40°C. 2 L of acetonitrile was added dropwise while continuing to raise the temperature to 55°C. The dropwise addition was completed in 5 minutes, and stirring was continued for 30 minutes. Rapid cooling down to 0°C. A large amount of product was precipitated, and the stirring was continued for 1 hour, and the product was obtained by filtration, and the solid was dried in a blast oven at 55° C. for 8 hours to obtain 183 g of idelaris crystal form R, whose X-ray powder diffraction pattern was as follows: figure 2 shown.

Embodiment 3

[0121] Example 3: Preparation of Idelaris Form R

[0122] In a 5L glass bottle, add 500g of idelaris amorphous solid, add 500ml of dichloromethane, 75ml of absolute ethanol, stir mechanically, cool to 0°C, add dropwise 4L of acetonitrile, dropwise add in 10 minutes, continue to Stir at 0°C for 30 minutes. The product was obtained by filtration, and the solid was baked in a blast drying oven at 55°C for 8 hours to obtain 462g of Idelaris crystal form R, and its X-ray powder diffraction pattern was as follows: Figure 9 shown.

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PUM

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Abstract

The invention relates to idelalisib crystal, a pharmaceutical composition comprising the idelalisib crystal, and a preparation method and application of the idelalisib crystal, and belongs to the technical field of pharmaceutical composition crystals. The invention particularly provides crystal R; under Cu-KAlpha irradiation, the crystal R has X-ray powder diffraction spectrum substantially shown as in figure 1, 2 or 9. The preparation method of the crystal R is simple, the form of the crystal is easy to control, production efficiency is significantly increased, and the crystal R is more suitable for industrial production. The crystal has improved hygroscopicity, chemical stability and preparation adaptability, as well as improved efficacy and safety.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical compound crystals, and specifically relates to a new crystal form of Idelaris, a pharmaceutical composition containing the crystal form, and a preparation method and application of the crystal form. Background technique [0002] Idelalisib, also known as Idelalisib. Idelalis is a phosphoinositide 3-kinase (PI 3-kinase) inhibitor originally developed by Icos Corporation and developed by Gilead Sciences. The drug was approved by the U.S. FDA in July 2014 for the treatment of 3 types of B-cell blood cancer: combined with rituximab for relapsed chronic lymphocytic leukemia (CLL), as a monotherapy for relapsed follicular B-cell non-Hodgkin Chickkin's lymphoma (FL) and relapsed small lymphocytic lymphoma (SLL). [0003] Although the crystal form of the pharmaceutical compound has been studied in the prior art, both the characteristics of the crystal form and the preparation method need to be co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/34A61K31/52A61P35/00A61P35/02
CPCC07B2200/13C07D473/34
Inventor 张晓林胡斌刘城铭乐洋黄璐胡慧任冰王伟
Owner HUBEI BIO PHARMA IND TECHCAL INST
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