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Preparation method of small-particle-size bosentan

A technology of bosentan and small particle size, which is applied in the field of preparation of small particle size bosentan, which can solve the problems of multiple quality control, dust pollution, prolonging the preparation process, etc., achieve a good working environment, reduce environmental pollution, and save micropowder The effect of programming

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

These crushing methods, for pharmaceutical preparations, will have a certain amount of dust pollution; and prolong the preparation process of the preparation, adding some risk factors to quality control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The first step 16g bosentan crude product is dissolved in 100ml dichloromethane, filter;

[0018] The filtrate obtained in the second step and the first step is cooled to 0°C, and maintained, and 180ml of 50% ethanol aqueous solution is added under stirring; the stirring speed is 220 rpm, and the rate of adding ethanol aqueous solution is 10ml / min. After the addition is completed, continue Stir for 4 hours;

[0019] The third step is to filter, wash the filter cake 3 times with 50% ethanol aqueous solution, use 10ml each time, and dry at 70°C. Debosentan fine product, the HPLC detection purity is 99.76%, the yield is 93.82%, and the D90 is 32.56 microns.

Embodiment 2

[0021] The first step dissolves 25g bosentan crude product in 100ml dichloromethane, filters;

[0022] The filtrate obtained in the second step and the first step is cooled to 5°C and maintained, and 300ml of 60% ethanol aqueous solution is added under stirring; the stirring speed is 250 rpm, and the rate of adding ethanol aqueous solution is 15ml / min. After the addition is completed, continue Stir for 5 hours;

[0023] The third step is to filter, wash the filter cake with 60% ethanol aqueous solution for 3 times, use 10ml each time, and dry at 70°C. Debosentan fine product, the HPLC detection purity is 99.86%, the yield is 92.43%, and the D90 is 24.38 microns.

Embodiment 3

[0025] The first step 20g bosentan crude product is dissolved in 100ml dichloromethane, filter;

[0026] The filtrate obtained in the second step and the first step is cooled to 2°C and maintained, and 250ml of 55% ethanol aqueous solution is added under stirring; the stirring speed is 238 rpm, and the rate of adding ethanol aqueous solution is 12ml / min. After the addition is completed, continue Stir for 4.5 hours;

[0027] The third step is to filter, wash the filter cake with 50-60% ethanol aqueous solution for 3 times, use 10ml each time, and dry at 75°C. Debosentan is a high-quality product with a purity of 99.96% by HPLC, a yield of 93.73%, and a D90 of 16.89 microns.

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PUM

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Abstract

The invention relates to a preparation method of small-particle-size bosentan, and belongs to the technical field of raw material medicine preparation. According to a purifying method of the small-particle-size bosentan, firstly, an bosentan crude product is dissolved in dichloromethane, and filtering is conducted; filter liquid is cooled to 0 to 5 DEG C, the temperature is maintained, and 50-60%ethanol water with volume 1.8-3 times of that of the solvent in the first step is added in a flowing mode; stirring speed is 220-250 rpm, the speed of adding the ethanol water in a flowing mode is 10-15 ml / min, and after flowing adding is completed, stirring is conducted continuously for 4-5 hours; filtering is conducted, 50-60% ethanol water is used for washing filter cake, and drying is conducted. The invention provides the preparation method of the small-particle-size bosentan. The prepared bosentan D90 can be controlled to be between 16.89 micrometers and 32.56 micrometers, and a raw material medicine which can be used directly is provided for an bosentan preparation.

Description

technical field [0001] The invention relates to a method for preparing bosentan 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 years ...

Claims

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Application Information

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IPC IPC(8): C07D239/52
CPCC07D239/52
Inventor 不公告发明人
Owner WEIHAI YUNRUI INFORMATION TECH CO LTD
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