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Setastine hydrochloride crystal form F and preparation method thereof

A technology of sstatastine hydrochloride crystal and interplanar spacing, which is applied in the fields of medicine and biology, can solve the problems such as no literature report on sstatine hydrochloride crystal form F, and achieves good solvent safety, good stability, and preparation technology. simple effect

Active Publication Date: 2012-04-18
回音必集团抚州制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There is no bibliographical report on Sestatastine hydrochloride crystal form F and preparation method at present

Method used

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  • Setastine hydrochloride crystal form F and preparation method thereof
  • Setastine hydrochloride crystal form F and preparation method thereof
  • Setastine hydrochloride crystal form F and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 Preparation of Sestatastine Hydrochloride Form F

[0030] Take 1.0g of stastatine hydrochloride raw material, add 5~10ml of 50% acetone water, stir and reflux for 10 minutes, the reflux temperature is not higher than 60 oC , cool down, keep 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC , Under the condition of vacuum degree less than 100Pa, dry under reduced pressure for more than 20 hours, and then pulverize. In diffraction angle (2θ / o ), interplanar spacing (d / ?) and abundance ratio (I / I O ) at 5.58 (15.82, 41), 8.48 (10.41, 22), 9.76 (9.05, 33), 16.24 (5.45, 32), 16.76 (5.28, 73), 18.08 (4.90, 32) , 18.60 (4.76, 38), 21.32 (4.16, 100), 23.26 (3.82, 23), 23.8 (3.73, 48), 26.46 (3.36, 22), 27.72 (3.21, 28), 28.4 (3.14, 22) Obvious characteristic absorption peaks, see attached f...

Embodiment 2

[0031] The preparation of embodiment 2 Sestatastine hydrochloride crystal form F

[0032] Take 1.0g of Sestatastine hydrochloride raw material, add 5~10ml of 50% ethanol water, and the temperature of the water bath is not higher than 60 oC Stir to dissolve, cool and keep for 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC , Dry under reduced pressure for more than 20 hours under the condition of vacuum degree less than 100Pa, and then crush. Gained sitastine hydrochloride crystal form FX-diffraction spectrum, infrared spectrogram and differential scanning calorimetry figure and attached figure 1 , attached figure 2 , attached image 3 Basically the same.

Embodiment 3

[0033] Embodiment 3 Preparation of Sestatastine Hydrochloride Form F

[0034] Take 1.0g of Sestatastine Hydrochloride raw material, add water 10~20ml, 60 oC water bath dissolve, 10 oC The following crystallization, the crystallization time is not less than 10 hours, after the crystallization finishes, suction filtration separates, obtains stastatine hydrochloride solid, at 40 o C~60 oC Dry it under reduced pressure for more than 20 hours, and then crush it. Gained sitastine hydrochloride crystal form FX-diffraction spectrum, infrared spectrogram and differential scanning calorimetry figure and attached figure 1 , attached figure 2 , attached image 3 Basically the same.

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Abstract

The invention discloses a setastine hydrochloride crystal form F, a preparation method and an application of the setastine hydrochloride crystal form F in drugs. The setastine hydrochloride crystal form F provided by the invention is simple in preparation process and excellent in stability. Compared with the prior art, a sample prepared according to the method has the advantages that the residual amount of solvents toluene and dimethylbenzene introduced in a synthesizing process can be efficiently reduced, the product purity is excellent, and the setastine hydrochloride crystal form F is very beneficial to industrial production.

Description

technical field [0001] The invention belongs to the fields of medicine and biology, and relates to a crystal form of an antihistamine drug stastatine hydrochloride, a preparation method and an application in drug development. Background technique [0002] Setastine Hydrochloride (Setastine Hydrochloride, foreign trade name: Loderix, domestic trade name produced by our company: Qiqi) is a highly efficient and safe antihistamine, which can effectively relieve acute and chronic urticaria, eczema dermatitis, Various symptoms caused by pruritus and allergic rhinitis. The anti-allergic effect has quick onset, strong effect, less dosage and long duration; no drowsiness and no cardiotoxicity. Sestatastine hydrochloride is a new generation of anti-allergic drug, which was successfully developed by Egis Pharmaceuticals Ltd in Hungary and first launched in Hungary in 1987, and then listed in Czechoslovakia, Nigeria, the United States, Japan, Canada and most European countries. Chemi...

Claims

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Application Information

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IPC IPC(8): C07D295/088A61K31/55A61P37/08
Inventor 王大冲郭廷富王健张恒毛金平
Owner 回音必集团抚州制药有限公司
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