V crystal form of Fasudil hydrochloride and preparation method and application thereof
A technology of fasudil hydrochloride and crystal form, which is applied to the V crystal form of fasudil hydrochloride and the fields of its preparation and use, and can solve the problem of no fasudil hydrochloride crystal form, poor purity, large number of impurities, etc. question
Active Publication Date: 2013-04-24
TIANJIN CHASE SUN PHARM CO LTD
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Problems solved by technology
[0005] Fasudil hydrochloride has a variety of preparation methods, but its final product usually has the characteristics of amorphous form, and Fasudil hydrochloride prepared by other methods has many defects such as large number of impurities and poor purity.
Through research, the present invention finds a new crystal form of Fasudil hydrochloride, which has a whiter appearance, higher purity than anhydrous, and a single impurity less than 1‰, which meets the relevant requirements of the U.S. Food and Drug Administration (FDA). , is extremely important to the preparation of high-quality medicines, and there is no research report on Fasudil Hydrochloride Form V in the prior art
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0034] Weigh 20.0 g of Fasudil hydrochloride, add 60 mL of n-butanol-water mixture (volume ratio 4:1), heat to 80°C, stir to dissolve, filter while hot, and cool the filtrate to room temperature naturally, and let it stand for 1 hour. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a white crystalline powder.
Embodiment 2
[0036] Weigh 20.0 g of Fasudil hydrochloride, add 150 mL of n-butanol-water mixture (volume ratio 17:3), heat to 50°C, stir to dissolve, filter while hot, and cool the filtrate to room temperature naturally, and let it stand for 3 hours. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a white crystalline powder.
Embodiment 3
[0038] Weigh 20.0 g of Fasudil hydrochloride, add 240 mL of n-butanol-water mixture (volume ratio 9:1), heat to 30°C, stir to dissolve, filter while hot, and cool the filtrate to room temperature naturally, and let it stand for 5 hours. A solid was precipitated, filtered, and dried in vacuum for about 24 hours to obtain a white crystalline powder.
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The invention belongs to the technical field of medicines, and in particular relates to a V crystal form of Fasudil hydrochloride and a preparation method and application thereof. For the V crystal form of the Fasudil hydrochloride, under Cu-Ka radiation and through X-ray powder diffraction represented by a 2 theta angle, the V crystal form has characteristic peaks at the wavelength of 6.260, 8.300, 14.020, 20.960, 23.860, 25.580 and 27.020. The preparation method provided by the invention ensures that the product has high purity and low impurity content, and is more suitable for industrial production. The invention also discloses application of the Fasudil hydrochloride in improving and preventing ischemic cerebrovascular disease brought by various causes.
Description
technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a new crystal form of fasudil hydrochloride and a preparation method thereof. The invention also relates to using the crystal form to improve and prevent ischemic cerebrovascular diseases caused by various causes Diseases, such as cerebral infarction, vertebrobasilar insufficiency, delayed cerebrovascular disease (DINDS) after subarachnoid hemorrhage, cerebral vasospasm after brain surgery and interventional therapy, transient ischemic attack (TIA), cerebral hemorrhage recovery period, neurology cerebral infarction and other cerebral ischemia-related diseases. Background technique [0002] Fasudil hydrochloride [hexahydro-1-(5-isoquinolinesulfonyl)-homopiperazine, Fasudil] is a new type of isoquinolinesulfonamide derivatives. Its molecular weight is 818.23 and its molecular formula is C 28 h 34 N 6 o 4 S 2 3HCl 7H 2 O: [0003] [0004] Fasudil hydrochlori...
Claims
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IPC IPC(8): C07D401/12A61K31/551A61P9/10
Inventor 张存彦孙长海李学洁姚小青吴秀锦
Owner TIANJIN CHASE SUN PHARM CO LTD