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Crystal form II of Apatinib mesylate as well as preparation method and application of crystal form II

A technology of apatinib mesylate and crystal form, which is applied in the field of mesylate, can solve the problems of apatinib mesylate instability, strong hygroscopicity, etc., and achieve excellent stability, Effect of high solubility and low hygroscopicity

Inactive Publication Date: 2016-07-27
SHANGHAI SUNTRONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The problem to be solved by the present invention is to solve the instability and strong hygroscopicity of the existing apatinib mesylate, which are unfavorable for its use in pharmaceutical processing

Method used

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  • Crystal form II of Apatinib mesylate as well as preparation method and application of crystal form II
  • Crystal form II of Apatinib mesylate as well as preparation method and application of crystal form II
  • Crystal form II of Apatinib mesylate as well as preparation method and application of crystal form II

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 to 6

[0032] Embodiments 1 to 6 Preparation of Apatinib mesylate salt II crystal form

[0033] Weigh 500 mg of apatinib mesylate raw material in a container, add solvents (analytical grade) according to Table 1 and heat, and keep stirring at the heating temperature for 2 hours. After filtering, the filtered solution was kept at the volatilization temperature to volatilize the solvent to obtain a white solid. Then the obtained solid was dried under reduced pressure for 12 hours to obtain the crystal form II of apatinib mesylate salt. Weigh and calculate its yield, and the results are shown in Table 1.

[0034] Table 1 Preparation of Apatinib mesylate salt II crystal form

[0035]

Embodiment 7 to 12

[0036] Embodiment 7 to 12 Preparation of Apatinib mesylate salt II crystal form

[0037] Weigh 1.0 g of apatinib mesylate raw material in a container, add solvents (analytical grade) according to Table 2 and heat, and keep stirring at the heating temperature for 2 hours. After filtering, the filtered solution was slowly cooled to room temperature, and a white solid was precipitated. Then it was filtered again, and the obtained solid was dried under reduced pressure for 12 hours to obtain the crystal form II of apatinib mesylate. Weighing calculates its yield, and the result is shown in Table 2.

[0038] Table 2 Preparation of Apatinib mesylate salt II crystal form

[0039]

Embodiment 13

[0040] Example 13 Characterization of Apatinib mesylate II crystal form by XRPD

[0041] The measurement of the X-ray powder diffraction (XRPD) spectrum is carried out at room temperature using a D8Advance X-ray diffractometer from Bruker, Germany. The specific collection information is as follows: The radiation source is Cu-Kα 1 Ray, scan range (2θ range) from 3° to 40°, scan speed 12° / min, scan step size 0.02, slit width 0.01. Samples were processed using glass slides pressed directly onto the test plate. Subsequent XRPD patterns all adopt similar measurement methods.

[0042] Determination of the XRPD spectrum of the Apatinib mesylate II crystal form prepared according to the method described in Example 1 has Characteristic Cu-Kα 1 Diffraction peaks, such as figure 1 shown. The error range of 2θ value is ±0.2. After testing, the error range of 2θ value can also be ±0.15. A specific list of characteristic X-ray diffraction peaks derived from this spectrum is shown in ...

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PUM

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Abstract

The invention provides a crystal form II of Apatinib mesylate. The crystal form II is characterized in that Cu-Kalpha 1 rays are adopted for radiation, X-ray powder diffraction represented by a 2theta angle has diffraction peaks when the 2theta angle is 5.02 degrees, 10.28 degrees, 11.13 degrees, 13.75 degrees, 15.65 degrees, 18.18 degrees, 20.35 degrees, 20.86 degrees, 21.58 degrees and 24.96 degrees, and an error range of a 2theta value is plus or minus 0.2. The crystal form II of Apatinib mesylate has the advantages of good stability, low hygroscopicity and high solubility.

Description

technical field [0001] The invention relates to the mesylate salt of apatinib, a derivative of nicotinamide, a molecule-targeted antitumor drug, in particular to the crystal form II of apatinib mesylate and its preparation method and application. Background technique [0002] Nicotinamide derivative Apatinib (Apatinib), molecular formula C 24 h 23 N 5 O, whose chemical name is N-[4-(1-cyanocyclopentyl)phenyl]-2-(4-pyridylmethyl)amino-3-pyridinecarboxamide, is a molecularly targeted antineoplastic drug. As a typical small molecule vascular endothelial growth factor tyrosine kinase inhibitor, it can be used to treat advanced non-small cell lung cancer, gastric cancer, liver cancer, breast cancer and other tumor diseases. [0003] Chinese invention patent CN101676267 discloses the above-mentioned nicotinamide derivative mesylate (molecular formula C 24 h 23 N 5 O·CH 4 o 3 S, preparation method and application as shown in formula (I). [0004] [0005] The nicotinami...

Claims

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Application Information

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IPC IPC(8): C07D213/82C07C309/04C07C303/32A61K31/444A61P35/00
CPCC07B2200/13C07D213/82
Inventor 任国宾弋东旭陈金姚
Owner SHANGHAI SUNTRONG BIOTECH
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