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Preparation method of small-particle-size macitentan

A technology of macitentan and small particle size, which is applied in the field of preparation of small particle size macitentan, can solve problems such as prolonging the preparation process, environmental pollution, etc., and achieves the advantages of reducing environmental pollution, improving the working environment, and eliminating the micronization procedure. Effect

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

AI Technical Summary

Problems solved by technology

The micronization of macitentan tablets in the preparation process will prolong the preparation process and cause certain pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the first step, 7g of macitentan crude product is dissolved in 100ml of isopropanol-n-heptane mixed solvent, and filtered; the preparation concentration is 0.07g / ml of macitentan solution; in isopropanol-n-heptane mixed solvent , the volume ratio of isopropanol-n-heptane is 1.6:1;

[0020] The second step The temperature of the filtrate obtained in the first step is lowered to 5°C, and maintained, and 80ml of acetone is added under stirring; the stirring speed is 200 rpm, and the rate of feeding acetone is 8 / min. After the addition is completed, continue to stir for 3 hours;

[0021] The third step is to filter, wash the filter cake with a mixed solvent of isopropanol-n-heptane, and dry it at 60°C. The refined product of macitentan has a purity of 99.87% by HPLC, a yield of 93.682%, and a D90 of 38.06 microns.

Embodiment 2

[0023] The first step is to dissolve 18g of macitentan crude product in 100ml of isopropanol-n-heptane mixed solvent, filter; prepare a concentration of 0.18g / ml of macitentan solution; in isopropanol-n-heptane mixed solvent , the volume ratio of isopropanol-n-heptane is 1.6:1;

[0024] The filtrate obtained in the second step and the first step is cooled to 15°C and maintained, and 120ml of acetone is added under stirring; the stirring speed is -230 rpm, and the speed of adding acetone is 12ml / min. After the addition is completed, continue to stir for 5 hours ;

[0025] The third step is to filter, wash the filter cake with a mixed solvent of isopropanol-n-heptane, and dry it at 50°C.

[0026] The refined product of macitentan has a purity of 99.96% by HPLC, a yield of 92.743%, and a D90 of 3.5 microns.

Embodiment 3

[0028] In the first step, 12g of macitentan crude product is dissolved in 100ml of isopropanol-n-heptane mixed solvent, and filtered; the preparation concentration is 0.12g / ml of macitentan solution; in the isopropanol-n-heptane mixed solvent , the volume ratio of isopropanol-n-heptane is 1.6:1;

[0029] Step 2 Cool the filtrate obtained in the first step to 10°C and maintain it, and add 100ml of acetone under stirring; the stirring speed is 220 rpm, and the rate of feeding acetone is 11ml / min. After the addition is completed, continue to stir for 4.5 hours;

[0030] The third step is to filter, wash the filter cake with a mixed solvent of isopropanol-n-heptane, and dry it at 55°C.

[0031] The refined product of macitentan has a purity of 99.97% by HPLC, a yield of 93.52%, and a D90 of 8.96 microns.

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Abstract

The invention relates to a preparation method of small-particle-size macitentan, and belongs to the technical field of raw material medicine preparation. According to the preparation method of the small-particle-size macitentan, firstly, an macitentan crude product is dissolved in an isopropanol-n-heptane mixed solvent, and filtering is conducted; then obtained filter liquid is cooled to 5 to 15 DEG C, the temperature is maintained, under stirring, acetone with volume 0.8-1.2 times of that of the solvent in the first step is added in a flowing mode, stirring speed is 200-230 rpm, the speed ofadding the acetone in a flowing mode is 8-12 ml / min, and after flowing adding is completed, stirring is conducted continuously for 3-5 hours; filtering is conducted, and drying is conducted at 50-60 DEG C. The invention provides the preparation method of the small-particle-size macitentan. The prepared macitentan D90 can be controlled to be between 3.5 micrometers and 38.06 micrometers, and a rawmaterial medicine which can be used directly is provided for an macitentan preparation.

Description

technical field [0001] The invention relates to a preparation method of macitentan with small particle size, and belongs to the technical field of raw material medicine preparation. Background technique [0002] Pulmonary arterial hypertension (PAH) is a rare disease that is very unfamiliar to the general public but extremely malignant. About 15 to 25 people in every million people will suffer from this disease. It can occur in any age and gender, usually more than 70% of the patients are young, and the incidence rate of women is about 2 times higher than that of men. The onset of the disease is insidious and the development is relatively slow. The patient's earliest symptoms are usually shortness of breath, fatigue, and palpitations during physical activity. As the disease progresses, patients may even experience chest pain, cough, hemoptysis, and syncope. If the correct diagnosis and targeted treatment cannot be obtained in time, most patients will die within 2 to 3 yea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/47
CPCC07D239/47
Inventor 不公告发明人
Owner WEIHAI YUNRUI INFORMATION TECH CO LTD
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