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Axitinib crystal form preparation method

A crystal form, axitinib technology, applied in the field of preparation of axitinib crystal form, can solve problems such as difficulties, dangers, and high solvent viscosity, and achieve the effect of low production equipment requirements, high safety factor, and easy operation and control

Active Publication Date: 2014-11-12
JIANGSU HANSOH PHARMA CO LTD
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The specific defect is that the solvent toluene and xylene used in method one, method two, method three and method four belong to the second-class solvents stipulated in the "Chinese Pharmacopoeia", and the maximum residue required in the product is 890ppm toluene and 2170ppm xylene. The temperature of the crystal is high (110-140°C), and the production in the chemical workshop is a dangerous operation, which requires high production equipment and operators; method 5 uses PEG-400, which has a high viscosity and is not easy to operate in mass production. The boiling point of the solvent is higher than 300°C, which makes it very difficult to remove the residual solvent in the product

Method used

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reference example 1

[0024] Reference Example 1: Refer to the preparation method of crystal form I provided by patent WO2006048751A1 to prepare axitinib crystal form I. The method is: the 6-[2- (Methylcarbamoyl)phenylsulfanyl]-3-E-[2-(pyridin-2-yl)vinyl]indazole (4.6 g) was slurried in 50 ml methanol at 50 °C, After 15 minutes, 50ml of water was added, the slurry was stirred well and allowed to cool to room temperature. The solid was collected by filtration, washed successively with 50 ml of water and 30 ml of ethyl acetate, and dried under high vacuum to obtain crystalline form I.

reference example 2

[0025] Reference Example 2: Refer to the preparation method of crystal form II provided by patent WO2006048751A1 to prepare axitinib crystal form II. The crystal form is hydrate.

reference example 3

[0026] Reference Example 3: Refer to the preparation method of ethyl acetate solvate provided by patent WO2006048751A1 to prepare axitinib ethyl acetate solvate (that is, the crystal form III described in the patent), and neutralize axitinib in ethyl acetate p-Toluenesulfonate derivative, the resulting solid was dried under vacuum at 65°C.

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Abstract

The invention relates to an axitinib crystal form preparation method. Specifically, XRD (X-ray diffraction) spectrum characteristic peaks of axitinib crystal form are shown as 2 theta angle (+ / -0.1), and located in the 8.8, 9.4, 11.9, 14.5, 15.1, 15.6, 19.0, 19.3, 20.3, 20.6, 21.6, 23.1, 24.1, 24.6, 24.9 and 26.0. The preparation method is as follows: putting axitinib or an axitinib solvate into a solvent, heating for slurrying, performing heat preservation, stirring, cooling to ambient temperature for granulation, filtering, and drying to obtain the target crystal form.

Description

technical field [0001] The present invention relates to a preparation method of axitinib crystal form, and the application of the preparation method in the fields of pharmacy and chemical industry. The characteristic peaks of the XRD pattern of the crystal form are represented by 2θ angles (±0.1), located at 8.8, 9.4, 11.9, 14.5, 15.1, 15.6, 19.0, 19.3, 20.3, 20.6, 21.6, 23.1, 24.1, 24.6, 24.9 and 26.0. Background technique [0002] Axitinib, chemical name: 6-[2-(methylcarbamoyl)phenylsulfanyl]-3-E-[2-(pyridin-2-yl)vinyl]indazole, structural formula is as follows: [0003] [0004] The use of axitinib and its pharmaceutically acceptable salts is disclosed in patent WO2001002369A2, the compound is a protein kinase receptor inhibitor and represents a synthetic, small molecule inhibitor of angiogenesis receptor signaling. [0005] In 2012, axitinib was launched in the United States, Japan, and European Union countries as a drug for advanced renal cell carcinoma after failur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/06
CPCC07B2200/13C07D401/06
Inventor 何雷张亮乔智涛刘昌会
Owner JIANGSU HANSOH PHARMA CO LTD
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