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Method for refining sulfonyl isoquinoline derivative

The technology of a sulfonyl isoquinoline and a refining method, which is applied in the field of medicine, can solve the problems of being unsuitable for mass production, long production cycle and high production cost, and achieve the effects of shortening production cycle, low production cost and good product quality.

Active Publication Date: 2013-02-27
SHANXI PUDE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] To sum up, in the existing patent literature, after the substitution reaction, purification by column chromatography is required. These methods are complicated to operate, have a long production cycle and high production cost, and are not suitable for mass production.

Method used

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  • Method for refining sulfonyl isoquinoline derivative
  • Method for refining sulfonyl isoquinoline derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Substitution reaction:

[0026] After sulfonation and chlorination, 5-sulfonylchloroisoquinoline was obtained in the reaction flask, and 356.0 ml of dichloromethane and 31.4 grams of 1,4-diazepane were added to the reaction flask, and the temperature was lowered to -5 ~0°C, 650 ml of methylene chloride solution containing 29.3 g of 5-sulfonylchloroisoquinoline was added dropwise, and the temperature was always controlled between -5 and 0°C during the dropping process. Then react for 3 hours under the condition of 0-5°C.

[0027] 2. Purification:

[0028] 1) After the substitution reaction is finished, add 150.0 milliliters of purified water to the obtained reaction solution, stir to fully mix the purified water with the above-mentioned solution, let stand to separate the layers, separate the water layer, and use 100.0 milliliters of dichloromethane to back-extract the water layer, Combine the organic layers.

[0029] 2) Below 30°C, the obtained organic layer was c...

Embodiment 2

[0036] 1. Substitution reaction:

[0037] After sulfonation and chlorination, 5-sulfonylchloroisoquinoline was obtained in the reaction flask, and 2.9 liters of dichloromethane and 259.2 grams of 1,4-diazepane were added to the reaction flask, and the temperature was lowered to -5 ~0°C, add dropwise 5.1 liters of dichloromethane solution containing 243.1 g of 5-sulfonylchloroisoquinoline, and keep the temperature between -5 and 0°C throughout the dropping process, and the dropwise addition is completed within 1 to 2 hours. Then react for 3 hours under the condition of 0-5°C.

[0038] 2. Purification:

[0039] 1) After the completion of the substitution reaction, add 1.2 liters of purified water to the obtained reaction solution, stir to fully mix the purified water with the above solution, leave to stand for stratification, separate the water layer, and use 0.9 liters of dichloromethane to back-extract the water layer, The organic layers were then combined.

[0040] 2) Belo...

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Abstract

The invention relates to a method for refining a sulfonyl isoquinoline derivative generally known as a Fasudil hydrochloride medicament for treating cerebral spasm caused by subarachnoid hemorrhage. The method of the invention comprises the steps of purification and refining and salification, wherein the step of purification comprises washing with water, concentrating, acidifying, extracting and crystallizing; and the step of salification and refining combines the Fasudil salification and subsequent refining of the prior art. The purification, refining and salification method of the invention has the advantages of simplifying operation flow, shortening production period, reducing production cost, improving product quality and bringing a great convenience to industrial production.

Description

technical field [0001] The invention relates to a method for refining a medicine for treating cerebral spasm caused by subarachnoid hemorrhage, specifically a medicine refining method for a sulfonylisoquinoline derivative, namely fasudil hydrochloride commonly known as fasudil hydrochloride, which belongs to the field of medicine. Background technique [0002] Fasudil hydrochloride is a sulfonylisoquinoline derivative, its English name is FasudilHydrochloride, its chemical name is hexahydro-1-(5-sulfonylisoquinoline)-1(H)-1,4-di Azepine hydrochloride, the molecular formula is C 14 h 17 N 3 o 2 S HCl, the chemical structure is as follows: [0003] [0004] Fasudil hydrochloride is a new type of intracellular calcium ion antagonist developed by Asahi Kasei Co., Ltd. of Japan. It has the effects of cerebral vasodilator and other effects. It is clinically used to treat cerebral spasm caused by subarachnoid hemorrhage. It was released in Japan in June 1995 marketed and ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12
Inventor 胡成伟解晓荣李立忠李润宝王勇张磊
Owner SHANXI PUDE PHARMA CO LTD
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