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New sunitinib malate crystal form and preparation method therefor

A malate and sunitinib technology, applied in the new sunitinib malate crystal form and its preparation field, achieves the effects of low thermal stability and good solubility

Inactive Publication Date: 2015-11-25
SHANGHAI SYNCORES TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, there are certain defects in the currently screened sunitinib malate crystal form

Method used

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  • New sunitinib malate crystal form and preparation method therefor
  • New sunitinib malate crystal form and preparation method therefor
  • New sunitinib malate crystal form and preparation method therefor

Examples

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Effect test

preparation example

[0029] In order to illustrate the present invention in more detail, the following preparation examples are given, but the scope of the present invention is not limited thereto.

[0030] The analytical detection condition of the present invention is as follows:

[0031] 1. DSC is measured by SDTQ600 of American TA Company, the test condition is 120ml / minN 2 , The heating rate is 10°C / min.

[0032] 2. X-ray powder diffraction data is measured by X′PertProMPD (Multi-Purpose Diffractometer), light tube type: EmpyreanXRDtubeCuLFFHR; voltage and current: 45kV, 40mA; goniometer: PW3050 / 60 vertical goniometer, radius 240mm; Slit: DS=2°, SS=1 / 2°, mask=15mm, RS=5.0mm; detector: X′Celerator super energy detector; scanning mode: continuous scanning; scanning range: 3°-40°2θ ; Counting time per step: 20s; total scanning time: 6min.

Embodiment 1

[0033] Example 1: Sunitinib Malate FormⅧ

[0034] Mix 100mg of sunitinib free base and 34mg of L-malic acid, add 4ml of tetrahydrofuran and 0.5ml of water, heat to 65°C to dissolve completely, and filter. The filtrate was cooled to 5°C, cooled to -25°C at a rate of 1°C / min after 2 minutes, maintained for 3 hours, filtered with suction, and vacuum-dried at 50°C for about 6 hours to obtain 93.5 mg of sunitinib malate FormⅧ.

Embodiment 2

[0035] Example 2: Sunitinib Malate FormⅧ

[0036] Mix 2.00g of sunitinib free base and 0.68g of L-malic acid, add 80ml of tetrahydrofuran and 10ml of water, heat to 65°C to dissolve completely, and filter. The filtrate was cooled to 5°C, cooled to -25°C at a rate of 1°C / min after 2 minutes, maintained for 3 hours, filtered with suction, and vacuum-dried at 50°C for about 6 hours to obtain 1.98 g of sunitinib malate FormⅧ.

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Abstract

The present invention relates to a new sunitinib malate crystal form and a preparation method therefor. The sunitinib malate is detected by Cu-Ka radiation to form an X-ray powder diffraction pattern, wherein characteristic peaks of Form VIII are at approximately 3.15 degree, 9.43 degree, 10.07 degree, 12.63 degree, 14.85 degree, 15.74 degree, 17.65 degree, 18.96 degree and 20.53 degree(2 theta). Characteristic peaks of Form IX are at approximately 3.09 degree, 7.63 degree, 9.15 degree, 9.63 degree, 12.16 degree, 12.84 degree, 15.21 degree, 16.13 degree, 18.36 degree, 18.93 degree, 22.47 degree and 27.39 degree(2 theta). The present invention further provides a method for preparing the Form VIII and the Form IX of the sunitinib malate. The sunitinib malate crystal form prepared by the preparation method is good in solubility, high in stability, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a new pharmaceutically acceptable crystal form of sunitinib malate and a preparation method thereof. technical background [0002] Sunitinib is represented by formula (I), and its chemical name is N-[2-(diethylamino)ethyl]-5-[-(5-fluoro-1,2-dihydro-2-oxo- 3H-indole-3-ylidene)methyl]-2,4-dimethyl-1H-pyrrole-3-carboxamide is a novel multi-targeted tyrosine kinase inhibitor (TKI). [0003] [0004] Polymorphism is defined as the ability of a substance to exist in two or more different crystal structures. Crystal form can affect different aspects of the solid-state properties of a drug, such as its solubility, stability, dissolution rate, crystallinity, bioavailability, and affect the preparation of pharmaceutical formulations and their properties. [0005] Therefore, in order to pursue better solubility, bioavailability or stability, a lot of screening work has been carried out for different crystal forms of sunitinib malate....

Claims

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Application Information

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IPC IPC(8): C07D403/06C07C59/245C07C51/41
CPCC07D403/06C07B2200/13
Inventor 不公告发明人
Owner SHANGHAI SYNCORES TECH INC
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