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Alpha crystal form of racecadotril and preparation method of alpha crystal form

A technology for racecadotril and crystal form, which is applied in the field of drug crystal form and preparation, can solve problems such as unreported crystal form, and achieve the effects of high crystal form purity, easy implementation and stable crystal form

Inactive Publication Date: 2015-02-18
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In documents such as WO2011116490A1, US5945548, and CN101768095A, the synthesis process of racecadotril was recorded, but its crystal form was not reported; therefore, the inventors conducted further research on the unreported crystal form of racecadotril. Research

Method used

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  • Alpha crystal form of racecadotril and preparation method of alpha crystal form
  • Alpha crystal form of racecadotril and preparation method of alpha crystal form
  • Alpha crystal form of racecadotril and preparation method of alpha crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Dissolve 40.0g of racecadotril in 200ml of absolute ethanol, heat in a water bath to 40°C, stir until completely dissolved, stop stirring, place the solution in a constant temperature water bath at 15°C, and when crystals begin to precipitate, then Placed at 0°C for crystallization, filtered, and dried with hot air circulation at 45°C for 6 hours to obtain 29.2 g of racecadotril α crystals with a purity of 99.6%.

[0033] The reflection angle 2θ of its X-ray powder diffraction pattern shows X-ray powder diffraction peaks at 4.3°, 8.7°, 13.2°, 16.8°, 17.8° and 20.0°. at 1135.19cm -1 、1551.46cm -1 、1644.73cm -1 、1687.57cm -1 、1731.35cm -1 and 3289.20cm -1 shows an infrared absorption peak.

Embodiment 2

[0035] Dissolve 40.0g of racecadotril in 400ml of 85% ethanol aqueous solution, heat in a water bath to 40°C, stir until completely dissolved, stop stirring, and place the solution in a constant temperature water bath at 20°C to stand still, when crystals begin to precipitate , and then placed at 5°C for crystallization, filtered, and dried with hot air circulation at 43°C for 6 hours to obtain 28.5 g of racecadotril α crystals with a purity of 99.4%.

[0036] The reflection angle 2θ of its X-ray powder diffraction pattern shows X-ray powder diffraction peaks at 4.3°, 8.7°, 13.3°, 16.7°, 17.8° and 20.0°. at 1135.09cm -1 、1551.92cm -1 、1644.24cm -1 、1687.22cm -1 、1731.71cm -1 and 3288.41m -1 shows an infrared absorption peak.

Embodiment 3

[0038] Dissolve 40.0g of racecadotril in 400ml of 70% ethanol aqueous solution, heat in a water bath to 45°C, stir until completely dissolved, stop stirring, put the solution in a constant temperature water bath at 25°C and let it stand, when crystals begin to precipitate , and then placed at 5° C. for crystallization, filtered, and dried with hot air circulation at 45° C. for 7 hours to obtain 30.4 g of racecadotril α crystals with a purity of 99.7%.

[0039] The reflection angle 2θ of its X-ray powder diffraction pattern shows X-ray powder diffraction peaks at 4.3°, 8.7°, 13.2°, 16.7°, 17.7° and 20.0°. at 1135.10cm -1 、1552.05cm -1 、1644.21m -1 、1687.28cm -1 、1731.50cm -1 and 3287.80cm -1 shows an infrared absorption peak.

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Abstract

The invention belongs to the technical field of crystal forms and preparation of drugs and particularly relates to an alpha crystal form of racecadotril and a preparation method of the alpha crystal form. The alpha crystal form of racecadotril is characterized in that the reflection angle 2theta shows X-ray powder diffraction peaks at sites of 4.2-4.3 degrees, 8.7-8.8 degrees, 13.2-13.3 degrees, 16.7-17.8 degrees, 17.7-17.8 degrees and 19.9-20.0 degrees and shows infrared absorption peaks at sites of 1135-1136cm<-1>, 1551-1553cm<-1>, 1644-1645cm<-1>, 1687-1688cm<-1>, 1731-1732cm<-1> and 3287-3290cm<-1> in an X-ray powder diffraction diagram. The preparation method comprises the following steps of dissolving racecadotril in a solvent, heating until racecadotril is dissolved, then standing still for crystallization, filtering, and drying. The prepared alpha crystal form of racecadotril is high in purity and stable; the preparation method is simple in process and easy to implement, the yield is 70%-80%, and the purify of the alpha crystal form is more than or equal to 99.0%.

Description

technical field [0001] The invention belongs to the technical field of drug crystal forms and preparation, and in particular relates to a racecadotril α crystal form and a preparation method thereof. Background technique [0002] Racecadotril, whose chemical name is N-[(R,S)-3-acetylmercapto-2-benzylpropionyl)]glycine benzyl ester, is a neprilysin inhibitor with selectivity and reversibility Inhibits enkephalinase, thereby protecting endogenous enkephalins from degradation, prolonging the physiological activity of endogenous enkephalins in the digestive tract, and is mainly used clinically for the treatment of acute diarrhea in children and adults. Its structural formula is as follows: [0003] [0004] Racecadotril, as an enkephalinase inhibitor, is a drug for the treatment of acute diarrhea developed and listed by French Bioprojet in 1993, with the trade name Tiorfan. [0005] In documents such as WO2011116490A1, US5945548, and CN101768095A, the synthesis process of r...

Claims

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Application Information

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IPC IPC(8): C07C327/32A61K31/265A61P1/12
Inventor 张涛李宗涛杨学谦刘印张爽任继波
Owner SHANDONG QIDU PHARMA
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