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Crystal form A of apatinib, and preparation method and application thereof

A technology of apatinib and crystal form, which is applied in the field of apatinib A crystal form and its preparation, can solve problems affecting the efficacy of drugs, and achieve excellent high-humidity stability and excellent thermal stability

Inactive Publication Date: 2018-07-06
SHANGHAI SUNTRONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These physical and chemical properties have a certain impact on the application of drugs, thereby affecting the efficacy of drugs

Method used

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  • Crystal form A of apatinib, and preparation method and application thereof
  • Crystal form A of apatinib, and preparation method and application thereof
  • Crystal form A of apatinib, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 to 9

[0036] Embodiments 1 to 9 Preparation of Apatinib Form A

[0037] Weigh 1g of apatinib raw material (purchased from Shanghai Hanxiang Biotechnology Co., Ltd., purity>98%) and place it in a container, add the solvents (analytical grade) in Table 1 respectively, and stir or shake at room temperature for 24h , and then centrifuged at 12,000 rpm for 5 minutes. The solid in the lower layer was vacuum-dried to obtain a white solid, which is the Apatinib A crystal form. Weigh and calculate its yield, and the results are shown in Table 1.

[0038] Table 1 Preparation of Apatinib Form A

[0039]

Embodiment 10

[0040] Example 10 Characterization of Apatinib Form A by XRPD

[0041] The measurement of the X-ray powder diffraction (XRPD) pattern 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 A crystal form prepared according to the method described in Example 1 has characteristic Cu-Kα at 2θ=11.69, 16.13, 17.13, 17.82, 20.74, 21.81, 23.51, 23.87, 27.01° 1 Diffraction peaks, such as figure 1 shown. The error range of 2θ value is ±0.2°. After testing, the error range of the 2θ value can also be ±0.15°.

[0043] A specific list of characteristic X-ray dif...

Embodiment 11

[0048] Example 11 Characterization of Apatinib Form A by Infrared Spectroscopy

[0049] Use the Nicolet-Magna FT-IR 750 infrared spectrometer of Nicolet Corporation of the United States to detect the infrared spectrum of the Apatinib A crystal form prepared according to the method described in Example 1 at room temperature, and the detection range is: 4000~350cm -1 . The obtained infrared spectrum is attached as figure 2 As shown, at 3351, 2235, 1650, 1589, 1511, 1255, 1135cm -1 There is a strong absorption peak. Detect the Apatinib A crystal form prepared according to the method described in Examples 2-9, the obtained infrared spectrum and the attached figure 2 The spectra shown are essentially the same.

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PUM

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Abstract

The invention provides a crystal form A of apatinib, and a preparation method and application thereof. The crystal form A is as shown in a formula (I) which is described in the specification. In an XRPD pattern of the crystal form A of apatinib, a diffraction peak occurs when the angle 2theta is equal to 11.69, 16.13, 17.13, 17.82, 20.74, 21.81, 23.51, 23.87 or 27.01 degrees, and the error range of the value of the 2theta is + / -0.2 degree. The crystal form A of apatinib provided by the invention has good high-temperature stability and high-humidity stability.

Description

technical field [0001] The invention relates to apatinib, a nicotinamide derivative of a molecular targeting anti-tumor drug, in particular to a crystal form A of apatinib, a preparation method and application thereof. 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 apatinib (as shown in formula (I)) [0004] [0005] The preparation method of the salt and the application thereof in antitumor drugs. However, CN101676267 does not disclose the s...

Claims

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Application Information

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IPC IPC(8): C07D213/82A61K31/444A61P35/00
CPCC07D213/82C07B2200/13
Inventor 任国宾朱彬弋东旭陈金瑶
Owner SHANGHAI SUNTRONG BIOTECH
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