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Fasudil crystal formation IV as well as preparation method and application thereof

A technology of fasudil hydrochloride and its crystal form, which is applied in the field of medicine and can solve problems such as flammability, unfriendly smell of n-butanol, and easy volatility

Active Publication Date: 2011-05-18
TIANJIN CHASE SUN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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.
[0006] The method currently adopted adopts systems such as methanol / ether. Ethyl ether is extremely volatile and has a special smell; it is extremely flammable, and methanol is poisonous. In severe cases, it will cause blindness or even death, which is not convenient for large-scale production; the normal butanol refining system adopted Butanol smells unfriendly

Method used

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  • Fasudil crystal formation IV as well as preparation method and application thereof
  • Fasudil crystal formation IV as well as preparation method and application thereof
  • Fasudil crystal formation IV as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1200mL of the dichloromethane solution of the substituent of 5-sulfonylchloroisoquinoline and homopiperazine contains about 200g of the substituent. After being decolorized by activated carbon, salted with hydrochloric acid, extracted and separated, 500mL of light yellow aqueous phase was separated, which contained Fasudil hydrochloride.

Embodiment 2

[0042] Get the aqueous phase solution obtained in Example 1, pour it into a 3L round-bottomed flask, add 1000mL of isopropanol, heat, start stirring, when the solution temperature reaches about 65°C, start vacuum distillation, along with the separation of isopropanol and water After the azeotrope is evaporated, the volume of the solution is continuously reduced, and then 500mL of isopropanol is added. When the aqueous solution is about 600mL, a large amount of solids appear. Cool naturally, filter at 25°C, and dry at 80°C to obtain Fasan hydrochloride Dier crystals.

Embodiment 3

[0044] Get the aqueous phase solution obtained in Example 1, pour it into a 3L round-bottomed flask, add 1000mL of isopropanol, heat, start stirring, when the solution temperature reaches about 65°C, start vacuum distillation, along with the separation of isopropanol and water After the azeotrope is evaporated, the volume of the solution is continuously reduced, and then 500mL of isopropanol is added. When the evaporated aqueous solution is about 600mL, a large amount of solids appear. Cool naturally, filter at 55°C, and dry at 80°C to obtain Fasan hydrochloride Dier crystals.

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Abstract

The invention particularly relates to a Fasudil crystal formation IV as well as a preparation method and application thereof, belonging to the technical field of medicines. For the Fasudil hydrochloride V crystal formation, Cu-Ka radiation is adopted, and X-ray powder represented by an angle of 2 theta is diffracted by angles of 6.320, 14.240, 14.460, 17.040, 22.640, 22.940, 25.400, 25.700 and 28.100 degrees, wherein the angle of 2 theta has a characteristic peak. The Fasudil hydrochloride crystal formation prepared with the preparation method provided by the invention has the advantages of high physical stability, high purity and the like when being stored and used at normal temperature and is further suitable for industrial production. The invention further discloses the application of the Fasudil hydrochloride in improving and preventing of ischemic cranial vascular diseases caused by various reasons.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a crystal form IV of fasudil hydrochloride and a preparation method and application thereof. The present invention also relates to using this crystal form to improve and prevent ischemic cerebrovascular diseases caused by various reasons, such as delayed cerebrovascular diseases caused by cerebral infarction, vertebrobasilar artery insufficiency, subarachnoid hemorrhage ( Cerebral vasospasm, transient ischemic attack (TIA), recovery period of cerebral hemorrhage, cerebral infarction and other cerebral ischemia-related diseases after brain surgery and interventional therapy. Background technique [0002] Fasudil [hexahydro-1-(5-isoquinolinesulfonyl)-homopiperazine, Fasudil] is a novel isoquinolinesulfonamide derivative. Its molecular weight is 327.83 and its molecular formula is C 14 h 17 N 30 2S HCl: [0003] [0004] Fasudil has a therapeutic effect on ische...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/12A61K31/551A61P9/10A61P9/00
Inventor 姚小青孙长海董凯张存彦贾萍王瑞卿
Owner TIANJIN CHASE SUN PHARM CO LTD
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