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Method for preparing fasudil hydrochloride

A technology of fasudil hydrochloride and sulfonyl chloride hydrochloride, which is applied in the field of medicine and achieves the effects of high yield, controllable quality and simple operation

Inactive Publication Date: 2015-02-25
南京亿华药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to effectively improve and control product quality and overcome difficulties encountered in industrial production, on the basis of combining patent literature reports, the present invention has carried out in-depth research on the synthesis process of Fasudil hydrochloride, including washing, hydrochloric acid extraction, Recrystallization and other post-processing steps to obtain a preparation method of Fasudil hydrochloride, which meets the needs of large-scale industrial production

Method used

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  • Method for preparing fasudil hydrochloride
  • Method for preparing fasudil hydrochloride
  • Method for preparing fasudil hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0037] The preparation of embodiment 1 Fasudil hydrochloride

[0038] (1) Add isoquinoline-5-sulfonic acid (60g, 0.287mol) into a 1000mL three-necked flask, add thionyl chloride (500ml, 6.893mol), and add 4mL of N,N-dimethylformamide dropwise , mechanically stirred, and heated to reflux for 6h. Generate hydrogen chloride and sulfur dioxide gas with 40% sodium hydroxide solution to absorb. Lower the temperature slightly, and distill off excess thionyl chloride under reduced pressure. When the temperature was lowered to room temperature, 160 mL of dichloromethane was added to the reaction flask and stirred for 30 minutes, cooled to below 20°C, filtered with suction, the filter cake was washed three times with dichloromethane, and dried under reduced pressure to obtain 61.9 g of white solid powder isoquinoline-5 -sulfonyl chloride hydrochloride.

[0039] (2) Add 454 mL each of water and dichloromethane to a 2000 mL three-necked flask, cool down to about 0°C, add isoquinoline-5...

Embodiment 2

[0042] The preparation of embodiment 2 Fasudil hydrochloride

[0043] (1) Add 0.6kg of isoquinoline-5-sulfonic acid and 5L of thionyl chloride into a 20L reactor, stir mechanically, then add 40mL of DMF, and reflux for 4.5 to 6 hours. After the reaction is completed, the temperature of the reaction solution is lowered to about 50-55°C, and after the thionyl chloride is evaporated under reduced pressure, the temperature is lowered to 20-30°C, and 1.6L of CH 2 Cl 2 , stirred, suction filtered, the filter cake was washed with dichloromethane, and dried under reduced pressure to obtain 0.705kg of isoquinoline-5-sulfonyl chloride hydrochloride.

[0044] (2) Add 4.5L of water and 4.5L of methylene chloride in a 20L reactor, stir mechanically, add 0.705kg of isoquinoline-5-sulfonyl chloride hydrochloride and 0.2kg of NaHCO 3 , the temperature is controlled not to exceed 10°C, and the pH value is adjusted to 7. After stirring and reacting for 30 minutes, let stand to separate layer...

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Abstract

The invention relates to a method for preparing fasudil hydrochloride. A fasudil hydrochloride synthetic technology is researched deeply. The method for preparing fasudil hydrochloride comprises aftertreatment steps of washing, hydrochloric acid extracting, recrystallizing and the like to obtain the fasudil hydrochloride, the single impurity content of the obtained fasudil hydrochloride finished product is lower than 0.02%, the content (high performance liquid chromatography (HPLC)) is higher than 99.95%, an aftertreatment technology is simple, a column chromatographic extraction method is not adopted, and the method has the advantages of high yield, controllable quality, simplicity in operation and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation process of a bulk drug, in particular to a preparation process of a fasudil hydrochloride bulk drug used for improving symptoms of ischemic cerebrovascular diseases caused by cerebral vasospasm after subarachnoid hemorrhage, and belongs to the field of medical technology . Background technique [0002] Subarachnoid hemorrhage (SAH) is an acute hemorrhagic cerebrovascular disease caused by rupture of blood vessels at the base of the brain or on the surface of the brain and spinal cord due to various etiologies. Blood directly flows into the subarachnoid space, which is called primary subarachnoid hemorrhage; in critical clinical cases, blood can also penetrate the brain tissue and flow into the subarachnoid space due to intraparenchymal, ventricular hemorrhage, epidural or subdural blood vessel rupture, etc. Cavity, called secondary subarachnoid hemorrhage, as well as bleeding caused by trauma. Patients with suba...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12
Inventor 杨鹏辉刘琴付新年
Owner 南京亿华药业有限公司
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