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Compound for treatment of respiratory system diseases and preparation method thereof

A technology for respiratory diseases and compounds, applied in respiratory diseases, organic chemistry methods, organic chemistry, etc., can solve problems such as differences in bioavailability, and achieve good stability, good fluidity and compressibility, and good solubility. Effect

Active Publication Date: 2016-12-07
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Different crystalline forms of the same drug may have significantly different bioavailability

Method used

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  • Compound for treatment of respiratory system diseases and preparation method thereof
  • Compound for treatment of respiratory system diseases and preparation method thereof
  • Compound for treatment of respiratory system diseases and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Take 10 g of crude erdosteine, add it to a mixed solution of 100 ml of methanol and petroleum ether (volume ratio 3:1) at a temperature of 30° C., stir at 40 rpm to dissolve all of it, and obtain an erdosteine ​​solution;

[0049] (2) After dissolving, add 0.005g of activated carbon, decolorize for 30 minutes, filter to obtain a clear solution;

[0050] (3) Keep stirring at a speed of 40rpm, and at the same time add 60ml of acetone and ethanol (2:1) mixed solution to the filtrate at a constant speed of 10ml / min. ℃, grow crystal for 4 hours;

[0051] (4) Cool down to 5°C at a rate of 5°C / hour, stir at a controlled speed of 50rpm for 2 hours, keep the temperature and let it stand for 5 hours, and white crystals are precipitated;

[0052] (5) Suction filtration, the filter cake was washed twice with a small amount of petroleum ether, and vacuum-dried at 35° C. to obtain 9.73 g of white erdosteine ​​compound crystals.

[0053] Measured by powder X-ray diffraction meth...

Embodiment 2

[0060] (1) Take 10 g of crude erdosteine, add it to a mixed solution of 40 ml of methanol and petroleum ether (volume ratio 5:1) at a temperature of 50° C., stir at 60 rpm to dissolve all of it, and obtain an erdosteine ​​solution;

[0061] (2) After dissolving, add 0.01g of activated carbon, decolorize for 20 minutes, filter to obtain a clear solution;

[0062] (3) Keep stirring at a speed of 60rpm, and at the same time, add 80ml of acetone and ethanol (3:1) mixed solution to the filtrate at a constant speed of 15ml / min. ℃, grow crystal for 2 hours;

[0063] (4) Cool down to 0°C at a rate of 15°C / hour, stir at a controlled speed of 90rpm for 0.5 hours, keep the temperature and let it stand for 8 hours, and white crystals are precipitated;

[0064] (5) Suction filtration, the filter cake was washed twice with a small amount of petroleum ether, and vacuum-dried at 40°C to obtain 9.78 g of white erdosteine ​​compound crystals.

[0065] Measured by powder X-ray diffraction meth...

Embodiment 3

[0072] (1) Take 10 g of crude erdosteine, add it to a mixed solution of 70 ml of methanol and petroleum ether (volume ratio 4:1) at a temperature of 40° C., stir at 50 rpm to dissolve all of it, and obtain an erdosteine ​​solution;

[0073] (2) When the solution is clear, add 0.008g of activated carbon, decolorize for 25 minutes, and filter to obtain a clear solution;

[0074] (3) Keep stirring at a speed of 50 rpm, and at the same time, add 70 ml of acetone and ethanol (2.5:1) to the filtrate at a constant speed of 12 ml / min. ℃, crystal growth for 3 hours;

[0075] (4) Cool down to 5°C at a rate of 10°C / hour, stir at a controlled speed of 70rpm for 1 hour, keep the temperature for 6 hours, and precipitate white crystals;

[0076] (5) Suction filtration, the filter cake was washed twice with a small amount of petroleum ether, and vacuum-dried at 40° C. to obtain 9.85 g of white erdosteine ​​compound crystals.

[0077] Measured by powder X-ray diffraction method, the X-ray po...

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Abstract

Belonging to the field of medical technology, the invention discloses a compound for treatment of respiratory system diseases and a preparation method thereof, and specifically discloses a new erdosteine compound and a preparation method thereof. The erdosteine compound crystal's X-ray powder diffraction spectrum represented by a diffraction angle of 2theta+ / -0.2 degrees shows characteristic diffraction peaks at the positions of 3.41 degrees, 6.51 degrees, 8.48 degrees, 9.91 degrees, 12.65 degrees, 21.89 degrees, 24.48 degrees, 26.15 degrees, 30.69 degrees, 33.24 degrees, 35.56 degrees, 36.09 degrees, 38.35 degrees and 39.40 degrees, and the X-ray powder diffraction spectrum obtained by Cu-Kalpha ray measurement is shown as figure 1. The erdosteine crystal provided by the invention is different from the existing technology, has good stability, good solubility, good flowability and compressibility, and can be mixed evenly with other auxiliary materials.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to a compound for treating respiratory diseases and a preparation method thereof, in particular to a new erdosteine ​​compound crystal and a preparation method thereof. Background technique [0002] Phlegm is the product of respiratory inflammation, which can irritate the respiratory mucosa, cause cough and asthma, and aggravate infection. When patients with acute and chronic bronchitis or chronic lung disease have respiratory failure, if the patient's sputum is too viscous or forms sputum plugs, it can block the airway and cause suffocation. Therefore, it is of great significance to use mucus sputum regulators to dissolve mucus sputum, make it thinner, lower its viscosity, accelerate the movement of mucous membranes and cilia in the respiratory tract, and improve the transport function. [0003] The currently marketed mucus regulators, such as bromhexine, sodium thioethanesulfonate, and carb...

Claims

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Application Information

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IPC IPC(8): C07D333/36A61P11/00A61P11/10
CPCC07B2200/13C07D333/36
Inventor 董雪菊郑杜明孙正校
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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