Preparation method of axitinib

A technology of axitinib and ethanol, which is applied in the field of preparation of raw materials, can solve the problems of excessive content uniformity, fluctuations, adverse reactions, etc., and achieve the effect of reducing the loss of materials

Inactive Publication Date: 2018-02-23
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if the particle size is too fine, electrostatic adsorption will occur, resulting in excessive content uniformity, and fluctuations in the content of ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, the first step 8g Axitinib crude product is dissolved in the mixed solvent of 100ml acetone and ethanol, adds 0.4g gac, stirs 1 hour, filters; Mixed solvent described in this step, the volume ratio of acetone and ethanol is 1 : 0.3;

[0024] Step 2 Under stirring, slowly add 60ml of 95% ethanol dropwise to the filtrate of the first step at a rate of 4ml / min. After the addition is complete, quickly cool the system to -8°C and continue stirring for 1 hour; the rate of stirring is 300r / min

[0025] The third step is filtered, and the filter cake is washed 3 times with the mixed solution of the first step acetone and ethanol, each with 10ml, and the D90 of axitinib is 100 microns, and the purity detected by high performance liquid chromatography is 99.97%, and the yield is 94.02 %.

Embodiment 2

[0026] Embodiment 2, the first step 16g Axitinib crude product is dissolved in the mixed solvent of 100ml acetone and ethanol, adds 0.8g gac, stirs 1 hour, filters; Mixed solvent described in this step, the volume ratio of acetone and ethanol is 1 : 0.6;

[0027] Under stirring in the second step, slowly add 120ml of 95% ethanol dropwise to the filtrate of the first step at a rate of 8ml / min. After the addition is complete, quickly cool the system to -3°C and continue stirring for 3 hours; the stirring speed is 380r / min;

[0028] The third step is filtered, and the filter cake is washed 3 times with the mixed solution of the first step acetone and ethanol, each with 12ml, and the D90 of axitinib is 120 microns, and the purity detected by high performance liquid chromatography is 99.99%, and the yield is 93.96 %.

Embodiment 3

[0029] Example 3, the first step 14g crude axitinib was dissolved in a mixed solvent of 100ml acetone and ethanol, added 0.7g activated carbon, stirred for 1 hour, and filtered; the volume ratio of acetone and ethanol was 1:0.5;

[0030] Under stirring in the second step, slowly add 90ml of 95% ethanol dropwise to the filtrate of the first step at a rate of 5ml / min. After the addition is complete, quickly cool the system to -5°C and continue stirring for 2 hours; the stirring rate is 350r / min ;

[0031] The third step is to filter, and the filter cake is washed 3 times with the mixed solution of acetone and ethanol in the first step, each time using 10ml, to obtain axitinib D 90 It is 112 microns, the purity detected by high performance liquid chromatography is 99.99%, and the yield is 94.16%.

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PUM

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Abstract

The invention relates to a method for refining axitinib, which belongs to the technical field of preparation of raw materials. The preparation method of axitinib of the present invention comprises the following steps: the crude product of axitinib is dissolved in a mixed solvent of acetone and ethanol, adding 5% gac of axitinib weight, stirring, and filtering; Slowly add 95% ethanol that is 0.6-1.2 times the volume of the first-step solution into the first-step filtrate dropwise, after the dropwise addition, quickly cool the system to -8°C to -3°C, and continue stirring; the third step is filtered to obtain the present invention product. The invention provides a high-purity axitinib bulk drug with a D90 of 100-120 microns. The process of the invention is simple and easy to operate, and is suitable for industrial production. The product purity of the invention can reach more than 99.95%.

Description

technical field [0001] The invention relates to a method for refining axitinib, which belongs to the technical field of preparation of raw materials. Background technique [0002] Axitinib, alias Axitinib, chemical name: N -Methyl-2-[3-(( E )-2-pyridin-2-yl-vinyl)-1 H -indol-6-ylsulfonyl]-benzamide. Axitinib is an antineoplastic drug, clinically mainly used in adult patients with advanced renal cell carcinoma (RCC) who have previously failed a tyrosine kinase inhibitor or cytokine therapy. Axitinib was developed by Pfizer and was approved by the FDA on January 27, 2012. There are 2 specifications of 1 mg tablet and 5 mg tablet. [0003] Axitinib is a white powder with a melting point of 218.4°C, slightly soluble in polyethylene glycol 400, slightly soluble in methanol or ethanol, very slightly soluble in acetonitrile, and almost insoluble in water. The solubility in pH 1.2 hydrochloric acid solution at 20°C is 0.8 mg / ml, and in pH 6.8 phosphate buffer solution is 0.2 mi...

Claims

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Application Information

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IPC IPC(8): C07D401/06
CPCC07D401/06
Inventor 孙爱梅
Owner WEIHAI GUANBIAO INFORMATION TECH
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