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Azelnidipine crystal form, preparation method for same and officinal composition thereof

A technology of Azhedipine and crystal form, which is applied in the field of medicine, can solve the problems of unfavorable production operation and high static electricity of Azhedipine α crystal form, and achieve the effect of small electrostatic interaction, simple production operation and good stability

Active Publication Date: 2013-10-23
QINGDAO HUANGHAI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the disadvantages in the prior art that the α-crystal form of Azeldipine has high static electricity and is unfavorable for production operation, the present invention provides a new crystal form of Azeldipine and its preparation method and pharmaceutical composition

Method used

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  • Azelnidipine crystal form, preparation method for same and officinal composition thereof
  • Azelnidipine crystal form, preparation method for same and officinal composition thereof
  • Azelnidipine crystal form, preparation method for same and officinal composition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Thoroughly mix 10 g of amorphous azedipine with 40 ml of toluene, and heat to 30-40°C. Then add 2 to 3 g of activated carbon, stir and filter, add 40 ml of cyclohexane to the filtrate while stirring, continue to stir and crystallize, filter and dry to obtain 9.5 g of the new crystal form of azedipine, with a yield of 95% and a melting point of 163.4°C.

[0024] Heating to 40-50°C, and performing the same operations as above to obtain 9.4 g of the new crystal form of azelnidipine, with a yield of 94% and a melting point of 162.1°C.

[0025] Heating to 50-60°C, and performing the same operations as above to obtain 9.4 g of the new crystal form of azelnidipine, with a yield of 94% and a melting point of 162.7°C.

[0026] The above test proves that the heating and dissolving temperature ranges from 30 to 60°C. The higher the heating temperature, the longer the required crystallization time, so the preferred temperature is 30-40°C.

Embodiment 2

[0028] Thoroughly mix 10 g of amorphous azedipine with 40 ml of toluene, and heat to 30-40°C. Then add 2 to 3 g of activated carbon, stir and filter, add 40 ml of cyclohexane to the filtrate while stirring, continue to stir and crystallize, filter and dry to obtain 9.5 g of the new crystal form of azedipine, with a yield of 95% and a melting point of 163.8°C.

[0029] Using 50ml of toluene and 50ml of cyclohexane each, the rest was the same as above to obtain 9.4g of the new crystal form of azelnidipine, with a yield of 94% and a melting point of 163.7°C.

[0030] Using 60ml each of toluene and cyclohexane, the rest was the same as above to obtain 9.3g of the new crystal form of azeldipine, with a yield of 93% and a melting point of 162.2°C.

[0031] The above experimental results show that: for 10 g of amorphous azedipine, the preferred dosage of toluene is 40-60 ml. Experimental studies have found that when 10g of azeldipine is mixed with 40-60ml of toluene, the concentrati...

Embodiment 3

[0033] Thoroughly mix 10 g of amorphous azedipine with 40 ml of toluene, and heat to 30-40°C. Then add 2 to 3 g of activated carbon, stir and filter, add 20 ml of cyclohexane to the filtrate while stirring, continue to stir and crystallize, filter and dry to obtain 8.9 g of the new crystal form of azedipine with a yield of 89% and a melting point of 164.1°C.

[0034] 40ml of cyclohexane was added, and the rest was performed as above to obtain 9.5g of the new crystal form of azeldipine, with a yield of 95% and a melting point of 163.1°C.

[0035] 80ml of cyclohexane was added, and the rest was the same as above to obtain 9.6g of the new crystal form of azeldipine, with a yield of 96% and a melting point of 162.9°C.

[0036] The above experimental results show that the volume ratio of cyclohexane to toluene is 1:2 to 2:1, preferably an equal volume ratio. Too little cyclohexane will cause the yield to decrease, and when it reaches 1:1, the new crystal form of azeldipine is almo...

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Abstract

The invention provides a novel azelnidipine crystal form, a preparation method for the same and an officinal composition thereof. The X-ray powder diffraction characteristic absorption peak value 2theta of the novel azelnidipine crystal form is 5.68, 11.33, 12.34, 13.18, 13.55, 15.00, 16.26, 18.16, 20.60, 21.50, 23.09, 23.66, 24.62 and 27.19. The preparation method for the novel azelnidipine crystal form includes the steps: mixing amorphous azelnidipine with methylbenzene according to amount ratio ranging from 1:4 to 1:6 (w / v) prior to heating, adding activated carbon with stirring and filtering, adding cyclohexane into filtrate with the amount ratio of the cyclohexane to the methylbenzene ranging from 1:2 to 2:1 (v / v), and obtaining the novel azelnidipine crystal form by means of crystallization, filtration and drying. The novel azelnidipine crystal form is durable in drug properties, small in static electricity, higher in stability, high in yield and suitable for mass production.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a new crystal form of azedipine, a preparation method thereof and a pharmaceutical composition. Background technique [0002] Hypertension is a common and frequently-occurring disease, and the number of patients is increasing year by year. Now it has become one of the main killers of human health. The antihypertensive drug azelindipine is a long-acting dihydropyridine calcium ion antagonist jointly developed by Japan Sankyo Co., Ltd. and Japan Ube Industries Co., Ltd. It was first listed in Japan in May 2003. [0003] The pharmacological action mechanism of Azedipine is that it has a strong L-type calcium channel antagonistic effect, which can reduce the free calcium concentration in vascular smooth muscle cells, dilate blood vessels, and lower blood pressure. Pharmacodynamic studies have shown that the antihypertensive effect of azedipine is mild and long-lasting. In additi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12A61K31/4427A61P9/10
Inventor 黄清华赵明媚李延顺毕文慧鲁大东纪存朋李永刚宋厚芳
Owner QINGDAO HUANGHAI PHARM CO LTD
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