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Preparation method of impurity W in cisatracurium besylate

A technology of cisatracurium besylate and impurities, which is applied in the field of impurities in cisatracurium besylate and cisatracurium besylate, which can solve the problems of unclear efficacy and side effects, and difficulties in impurity W, etc. problem, to achieve the effect of simple preparation method, high purity, and promotion of research

Active Publication Date: 2019-09-20
江苏盈科生物制药有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no report on the relevant research on impurity W, and the impact of the content of impurity W on the efficacy and side effects of cisatracurium besilate is not clear. Therefore, it is necessary to control the presence of impurity W in cisatracurium besilate. content in curium ammonium; in order to quantitatively detect and analyze the content of impurity W in cisatracurium besylate product, it is necessary to obtain impurity W with higher purity, because the content of impurity W in cis atracurium besylate The content is low, and it is extremely difficult to purify high-purity impurity W from cisatracurium besylate. Therefore, how to prepare impurity W with higher purity is extremely important for the research on impurity W

Method used

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  • Preparation method of impurity W in cisatracurium besylate

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preparation example Construction

[0030] A kind of preparation method of impurity W in cisatracurium besylate, the structure of impurity W is as shown in formula (I),

[0031] Formula (I):

[0032] The preparation method of impurity W comprises the steps:

[0033] A. Get 1,5-pentanediol, glacial acetic acid, and catalyst to react to obtain a reaction solution; wherein the catalyst is p-toluenesulfonic acid, and the molar ratio of 1,5-pentanediol, glacial acetic acid and catalyst is 1: 1.4~1.6:0.4~0.6; During the reaction process, continuously feed boiling n-hexane into the reaction system (for example, n-hexane can be heated to 70-80°C) to reflux and divide water (the boiling n-hexane enters the reaction system to During the process of external circulation of the system, the water generated in the reaction system will be taken out to promote the positive progress of the reaction. When the n-hexane with water is discharged from the system, the water will be removed through the liquid separator first, and the...

Embodiment 1

[0045] A kind of preparation method of impurity W in cisatracurium besylate, the structure of impurity W is as shown in formula (I),

[0046] Formula (I):

[0047] The preparation method of impurity W comprises the steps:

[0048] A. Get 1,5-pentanediol, glacial acetic acid, and catalyst to react to obtain a reaction solution; wherein the catalyst is p-toluenesulfonic acid, and the molar ratio of 1,5-pentanediol, glacial acetic acid and catalyst is 1: 1.4:0.4; During the reaction process, continuously feed boiling n-hexane into the reaction system (for example, the n-hexane can be heated to 70°C) for reflux and water separation. After the reaction is completed, the boiling n-hexane is discharged from the system and no longer enters Reaction system, thereby abandoning n-hexane;

[0049] B. Add the mixed solution of water and n-hexane to the reaction solution, leave to stand for layering after stirring for liquid separation, discard the n-hexane layer solution, and collect t...

Embodiment 2

[0056] A kind of preparation method of impurity W in cisatracurium besylate, the structure of impurity W is as shown in formula (I),

[0057] Formula (I):

[0058] The preparation method of impurity W comprises the steps:

[0059] A. Get 1,5-pentanediol, glacial acetic acid, catalyzer to react, obtain reaction liquid; Wherein catalyzer is p-toluenesulfonic acid, the mol ratio of 1,5-pentanediol, glacial acetic acid and catalyzer is 1: 1.6:0.6; During the reaction process, continuously feed boiling n-hexane into the reaction system (for example, the n-hexane can be heated to 80°C) for reflux and water separation. After the reaction is completed, the boiling n-hexane is discharged from the system and no longer enters Reaction system, thereby abandoning n-hexane;

[0060] B. Add the mixed solution of water and n-hexane to the reaction solution, leave to stand for layering after stirring for liquid separation, discard the n-hexane layer solution, and collect the water layer so...

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Abstract

The invention discloses a preparation method of an impurity W in cisatracurium besylate, and belongs to the technical field of synthesis of chemical substances. The preparation method includes the following steps: A, taking and reacting 1,5-pentanediol, glacial acetic acid and a catalyst to obtain a reaction solution; B, adding water and n-hexane to the reaction solution, performing stirring and liquid separation, and collecting the obtained aqueous layer solution; C, washing the aqueous layer solution with n-hexane, and collecting the washed aqueous layer solution; D, extracting the aqueous layer solution with dichloromethane, and collecting the dichloromethane layer solution; E, adding a drying agent to the dichloromethane layer solution, and filtering and concentrating the obtained solution to obtain 1,5-pentanediol monoacetate; and F, reacting the 1,5-pentanediol monoacetate with the impurity A in cisatracurium besylate, adding a solvent, stirring and filtering the obtained solution to obtain impurity W crystals, and drying the impurity W crystals to obtain the final product impurity W. The impurity of the prepared cisatracurium besylate is high, the preparation method is simple, and the prepared impurity W can be directly used in the quantitative detection process of the impurity W in the cisatracurium besylate as a standard.

Description

technical field [0001] The invention relates to cisatracurium besylate, in particular to an impurity in cisatracurium besylate, and belongs to the technical field of chemical substance synthesis. Background technique [0002] Cisatracurium besylate, molecular formula C 53 h 72 N 2 o 12 .2(C 6 h 5 o 3 S); C 65 h 82 N 2 o 18 S 2 , is a chemical drug and the latest generation of muscle relaxants. Compared with the current main clinical muscle relaxant anesthetics, cisatracurium besylate has the characteristics of metabolism through non-hepatic and non-renal pathways and cardiovascular stability and muscle relaxant effect. It is 3 times stronger than atracurium and has no cardiovascular side effects. Cisatracurium besylate is mainly suitable for general anesthesia, and can be widely used in endotracheal intubation, liver and kidney dysfunction, cardiovascular surgery and elderly and pediatric patients. Since the drug was first launched in the UK in 1996, it has grad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20C07C303/32C07C309/29
CPCC07D217/20
Inventor 李海黄芳刘世普赵世超
Owner 江苏盈科生物制药有限公司
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