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Purification method of small-grain size nilotinib

A purification method and small particle size technology, applied in the direction of organic chemistry, etc., can solve problems such as environmental pollution, and achieve the effect of reducing environmental pollution, eliminating micronization procedures, and improving working environment.

Inactive Publication Date: 2018-09-28
WEIHAI YUNRUI INFORMATION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process of micronization will cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The first step is to dissolve 10g of nilotinib in 100ml of ethyl acetate to prepare a solution with a concentration of 0.1g / ml;

[0016] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0017] In the third step, the filtrate obtained in the second step is cooled to -5°C and maintained, and 100ml of 70% ethanol aqueous solution is added under stirring; the stirring speed is 220 rpm, and the rate of adding ethanol aqueous solution is 6ml / min. After the addition is completed, Continue stirring for 3 hours;

[0018] The fourth step is to filter, wash the filter cake with 70% ethanol aqueous solution, and dry to obtain the fine product of nilotinib. The HPLC detection purity is 99.36%, the yield is 92.38%, and the D90 is 48.61 microns.

Embodiment 2

[0020] The first step is to dissolve 21g nilotinib in 100ml ethyl acetate; prepare a solution with a concentration of 0.21g / ml;

[0021] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0022] The third step is to cool the filtrate obtained in the second step to 5°C and maintain it, and add 200ml of 50% ethanol aqueous solution under stirring; the stirring speed is 260 rpm, and the rate of adding ethanol aqueous solution is 10ml / min. After the addition is completed, continue Stir for 5 hours;

[0023] The fourth step is to filter, wash the filter cake with 50% ethanol aqueous solution, and dry to obtain nilotinib fine product. The purity of nilotinib detected by HPLC is 99.86%, the yield is 92.01%, and the D90 is 26.47 microns.

Embodiment 3

[0025] The first step is to dissolve 16g of nilotinib in 100ml of ethyl acetate; prepare a solution with a concentration of 0.16g / ml;

[0026] Step 2 Add 1g of activated carbon to the solution in the first step, stir, add 10ml of absolute ethanol, and filter;

[0027] The third step is to cool the filtrate obtained in the second step to 0°C and maintain it, and add 150ml of 60% ethanol aqueous solution under stirring; the stirring speed is 248 rpm, and the rate of adding ethanol aqueous solution is 8ml / min. After the addition is completed, continue Stir for 4.5 hours;

[0028] The fourth step is to filter, wash the filter cake with 60% ethanol aqueous solution, and dry to obtain the fine product of nilotinib. The HPLC detection purity is 99.84%, the yield is 93.68%, and the D90 is 29.21 microns.

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Abstract

The invention relates to a purification method of small-grain size nilotinib, and belongs to the technical field of crude drug preparation. According to the technical scheme, firstly, a nilotinib ethyl acetate solution is prepared, then activated carbon and absolute ethyl alcohol are added for filtering, and through the steps of cooling, fed-batch of 50-70% ethanol water, stirring speed controlling and the like, the small-grain size nilotinib is prepared. The small-grain size nilotinib obtained through the method can be directly used for preparation technologies, and thus the requirements of the different technologies for the crude drug can be met.

Description

technical field [0001] The invention relates to a method for purifying nilotinib with small particle size, and belongs to the technical field of preparation of raw materials. Background technique [0002] Nilotinib is an antineoplastic drug, mainly used clinically to treat chronic myelogenous leukemia resistant to Gleevec (imatinib). It is a powerful and precise second-generation tyrosine kinase inhibitor, which can effectively treat patients with drug-resistant or intolerant chronic myeloid leukemia. [0003] Nilotinib is an insoluble drug, and its solubility in water is 0.2ug / ml. In order to ensure the bioavailability of the original drug, Novartis uses micronized nilotinib to increase the dissolution of the main drug. However, the process of micronization will cause environmental pollution. Contents of the invention [0004] Aiming at the deficiencies of the prior art, the present invention provides a method for purifying nilotinib with small particle size, so as to a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14
CPCC07D401/14
Inventor 孙学胜
Owner WEIHAI YUNRUI INFORMATION TECH CO LTD
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