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Refining method of regorafenib

A technology of regorafenib and a refining method, applied in the refining field of regorafenib, can solve the problems of restricting practical application, low purity, unpredictable trace impurities in products, etc., and achieves the effects of reducing adverse reactions and improving purity

Inactive Publication Date: 2020-07-14
西安百宁医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As a drug, the low purity greatly restricts its practical application, and there are many existing methods for purifying compounds, and the purification methods combined by these methods are countless, but the unavoidable trace impurities in the products obtained by different purification methods are not. Unpredictable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 20g of regorafenib and place it in a flask, add 500ml of 80% acetone aqueous solution, water bath temperature 30-50°C, heat to make it all dissolve, add activated carbon, the amount of activated carbon is 5% of the mass of regorafenib %, then heat and filter (use suction filtration), collect the filtrate and let it stand to room temperature, place the filtrate in a 0-5°C environment for recrystallization (you can add seeds, stir and crystallize or stand for crystallization), and suction filter The filter cake was collected, and the obtained filter cake was vacuum-dried at room temperature to obtain the product (yield: 89.6%, related substances: 0.06%, purity: 99.94%, melting point: 206.0-207.5°C (decomposition when melting)).

Embodiment 2

[0022] Weigh 20g of regorafenib and place it in a flask, add 600ml of 80% ethanol aqueous solution, water bath temperature 30-50°C, heat to make it all dissolve, add activated carbon, the amount of activated carbon added is 5% of the mass of regorafenib. %, then heat and filter (use suction filtration), collect the filtrate and let it stand to room temperature, place the filtrate in a 0-5°C environment for recrystallization (you can add seeds, stir and crystallize or stand for crystallization), and suction filter The filter cake was collected, and the obtained filter cake was vacuum-dried at room temperature to obtain the product (yield: 83.6%, related substances: 0.10%, purity: 99.90%, melting point: 206.0-207.5°C (decomposition when melting)).

Embodiment 3

[0024] Weigh 20g of regorafenib and place it in a flask, add 550ml of 60% ethanol aqueous solution, water bath temperature 30-50°C, heat to make it all dissolve, add activated carbon, the amount of activated carbon is 5% of the mass of regorafenib %, then heat and filter (use suction filtration), collect the filtrate and let it stand to room temperature, place the filtrate in a 0-5°C environment for recrystallization (you can add seeds, stir and crystallize or stand for crystallization), and suction filter The filter cake was collected, and the resulting filter cake was vacuum-dried at room temperature to obtain the product (yield: 87.1%, related substances: 0.08%, purity: 99.92%, melting point: 206.0-207.5°C (decomposes when melting)).

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Abstract

The invention relates to a refining method of regorafenib. The preparation method comprises the following specific steps: (1) heating and dissolving regorafenib by using a solvent at the heating temperature of 20-60 DEG C, wherein the volume-mass ratio of the solvent to the regorafenib is less than or equal to 40: 1; wherein the unit of the solvent is g, and the unit of the regorafenib is g; (2) adding activated carbon, wherein the adding amount of the activated carbon is 2-6% of the mass of the regorafenib; (3) heating for decarburization, and then performing hot filtration; and (4) performing standing on a filtrate to room temperature, crystallizing in an environment of -20 to 30 DEG C, filtering, and collecting a filter cake to obtain the product. The method has the beneficial effects that the purity of the regorafenib is greatly improved, and adverse reactions caused by the existence of impurities are reduced.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for refining regorafenib. Background technique [0002] Regorafenib (regorafenib), the chemical name is 4-[4-({[4-chloro-3-(trifluoromethyl)phenyl]carbamoyl}amino)-3-fluorophenoxy]-N -Methylpyridine-2-carboxamide, developed by Bayer Healthcare in Germany, approved by the FDA in the United States, with a trade name of Stivarga. This product can inhibit a variety of kinases that promote the growth of cancer tissue, including VEGFR1-2, PDGFR-β, FGFR1 and KIT, etc., thereby inhibiting the formation of tumor angiogenesis and the proliferation of tumor cells, and is clinically suitable for the treatment of metastatic colorectal cancer . Its chemical structural formula is as follows: [0003] . [0004] As a drug, the low purity greatly restricts its practical application, and there are many existing methods for purifying compounds, and the purification methods combined by t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/81
CPCC07D213/81
Inventor 李晶红
Owner 西安百宁医药科技有限公司
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