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Purifying method of small-particle-size ambrisentan

A technology of ambrisentan and purification method, which is applied in the field of purification of ambrisentan with small particle size, can solve the problems of diffusion, environmental pollution, prolonging the preparation process, etc., achieve a good working environment, reduce environmental pollution, and save the cost of micronization procedures Effect

Inactive Publication Date: 2019-02-12
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process of vermicelli, first, prolongs the preparation process, and second, the particles formed in the vermicelli process will diffuse into the surrounding air, causing environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The first step is to dissolve 14g of ambrisentan crude product in 100ml of ethyl acetate, and filter; prepare a solution with a concentration of 0.14g / ml of ambrisentan;

[0016] The second step Add 1g of activated carbon to the first step solution, stir for 1.5 hours, and filter;

[0017] The filtrate obtained in the second step of the third step is cooled to -5°C, and maintained, and 150ml of 60% ethanol aqueous solution is added under stirring; the stirring speed is 230 rpm, and the rate of adding ethanol aqueous solution is 8ml / min. After the addition is completed, Continue stirring for 4 hours;

[0018] The fourth step is to filter, wash the filter cake 3 times with 60% ethanol aqueous solution, use 8ml each time, and dry at 80°C. The high-quality product of ambrisentan was obtained, the purity by HPLC was 99.56%, the yield was 93.38%, and the D90 was 40.61 μm.

Embodiment 2

[0020] The first step is to dissolve 26g of ambrisentan crude product in 100ml of ethyl acetate, and filter; prepare a solution of ambrisentan with a concentration of 0.26g / ml;

[0021] The filtrate obtained in the second step and the first step is cooled to 5°C, and maintained, and 300ml of 50% ethanol aqueous solution is added under stirring; the stirring speed is 270 rpm, and the rate of adding ethanol aqueous solution is 15ml / min. After the addition is completed, continue Stir for 5 hours;

[0022] The third step is to filter, wash the filter cake with 50% ethanol aqueous solution for 3 times, use 10ml each time, and dry at 80°C. The high-quality product of ambrisentan was obtained, the purity by HPLC was 99.86%, the yield was 92.43%, and the D90 was 24.38 μm.

Embodiment 3

[0024] The first step is to dissolve 17g of ambrisentan crude product in 100ml of ethyl acetate, and filter; prepare a solution of ambrisentan with a concentration of 0.17g / ml;

[0025] The filtrate obtained in the second step and the first step is cooled to 0°C, and maintained, and 220ml of 55% ethanol aqueous solution is added under stirring; the stirring speed is 250 rpm, and the rate of adding ethanol aqueous solution is 11ml / min. After the addition is completed, continue Stir for 4.5 hours;

[0026] The third step is to filter, wash the filter cake with 55% ethanol aqueous solution for 3 times, use 9ml each time, and dry at 80°C. The refined product of ambrisentan was obtained, with a purity of 99.76% by HPLC, a yield of 92.73%, and a D90 of 27.41 μm.

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Abstract

The invention relates to a purifying method of small-particle-size ambrisentan, and belongs to the technical field of raw material medicine preparation. According to the technical scheme, firstly, anambrisentan crude product is dissolved in ethyl acetate, then temperature is reduced to -5 to 5 DEG C, and under stirring, 50-60% ethanol water with volume 1.5-3 times of that of the solvent in the first step is added in a flowing mode; stirring speed is 230-270 rpm, the speed of adding the ethanol water in a flowing mode is 8-15 ml / min, and after flowing adding is completed, stirring is conductedcontinuously for 4-5 hours; filtering is conducted, 50-60% ethanol water is used for washing filter cake, and drying is conducted. The invention provides a preparation method of the small-particle-size ambrisentan. A raw material medicine which can be used directly is provided for an ambrisentan preparation, environmental pollution is reduced, and a well working environment is provided for preparation workers.

Description

technical field [0001] The invention relates to a method for purifying ambrisentan with small particle size, and belongs to the technical field of raw material medicine preparation. Background technique [0002] Ambrisentan, chemical name 2-(4,6-dimethylpyrimidin-2-yl)oxy-3-methoxy-3,3-diphenylpropionic acid, developed by GlaxoSmithKline, trade name VOLIBRIS (VOLIBRIS). [0003] Ambrisentan Tablets is a specific endothelin receptor A (ETA receptor) inhibitor drug, the specifications of the film-coated tablets of this drug are 5 and 10 mg / tablet, and it was approved by the FDA for marketing in June 2007. The drug can prevent excessive contraction of blood vessels by acting on endothelin and its receptors whose functions have changed in patients with pulmonary arterial hypertension, thereby alleviating disease symptoms, improving the quality of life and survival status of PAH patients. Ambrisentan is insoluble in water, Chinese patent 201410668103.5, adopts micronization pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/34
CPCC07D239/34
Inventor 不公告发明人
Owner WEIHAI GUANBIAO INFORMATION TECH
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