Preparation method for S-carvedilol

A technology of reaction kettle and ethylamine, applied in the field of preparation of S-carvedilol, can solve the problems of low conversion rate of S-epoxy carbazole, hinder the crystallization and purification of product S-carvedilol, etc., so as to improve the conversion rate. efficiency, continuous production, and low energy consumption

Inactive Publication Date: 2015-05-06
JIANGSU SUNAN PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] If the molar ratio of 2-(2-methoxyphenoxy)ethylamine and S-epoxycarbazole is low, the conversion rate of S-epoxycarbazole will be low
But if increase the charging capacity of 2-(2-methoxyphenoxy)ethylamine, the transformation rate of S-epoxycarbazole can be improved, but redundant 2-(2-methoxyphenoxy) in the system ) ethylamine will hinder the crystallization and purification of the product S-carvedilol

Method used

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  • Preparation method for S-carvedilol
  • Preparation method for S-carvedilol
  • Preparation method for S-carvedilol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The qualitative and quantitative detection method of the reaction substrate and product is: using Kromasil C 18 Column (12.5cm×4.6mm×5μm), mobile phase: acetonitrile: phosphate buffer (pH 2) (35:65); UV detection wavelength 240nm; flow rate: 1.0mL / min; column temperature 55°C.

[0024] S-epoxycarbazole, 2-(2-methoxyphenoxy)ethylamine (molar ratio 1:1) and solvent ethanol were pumped into the reaction kettle, heated to a reaction temperature of 80°C, and stirred vigorously for 1 hour. Pump the reaction solution from the bottom of the reaction tank into the middle of the rectification tower, heat it to 90°C for rectification, and separate the product, light ethanol and unreacted 2-(2-methoxyphenoxy)ethylamine at the top of the tower Condensed and refluxed into the reaction kettle, the crude heavy component flowed out from the bottom of the tower into the crystallization kettle, added ethyl acetate and recrystallized at 0°C for 30h to obtain the product. See Table 1 for t...

Embodiment 2

[0026] Reaction substrate and product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar ratio and each operating parameter are as follows:

[0027] S-epoxycarbazole, 2-(2-methoxyphenoxy)ethylamine (molar ratio 1:12) and solvent ethanol were pumped into the reaction kettle, heated to a reaction temperature of 30°C, and stirred vigorously for 1 hour. Pump the reaction solution from the bottom of the reaction tank into the middle of the rectification tower, heat it to 150°C for rectification, and separate the product, light ethanol and unreacted 2-(2-methoxyphenoxy)ethylamine at the top of the tower Condensed and refluxed into the reaction kettle, the heavy component crude product flowed out from the bottom of the tower into the crystallization kettle, added ethyl acetate and recrystallized at 40°C for 5h to obtain the product. See Table 1 for the results of the conversion rate...

Embodiment 3

[0029] Reaction substrate and product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar ratio and each operating parameter are as follows:

[0030] Pump S-epoxycarbazole, 2-(2-methoxyphenoxy)ethylamine (molar ratio 1:6.5) and solvent ethanol into the reaction kettle, heat to the reaction temperature of 55°C, and vigorously stir the reaction for 5.5h , the reaction solution is pumped from the bottom of the reaction tank into the middle of the rectification tower, heated to 120°C for rectification, and the product is separated, light ethanol and unreacted 2-(2-methoxyphenoxy)ethylamine The top is condensed, and refluxed into the reaction kettle, the crude heavy component flows out from the bottom of the tower into the crystallization kettle, and ethyl acetate is added to carry out recrystallization at 20°C for 18h to obtain the product. See Table 1 for the results of the conve...

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Abstract

The invention discloses a preparation method for S-carvedilol, which comprises the processes of product reaction, product rectification separation and recrystallization. Compared with the prior art, the preparation method adopts a reaction-rectification-crystallization continuous coupling process so that a reaction product is continuously and timely separated from a reaction system, the influence of excessive 2-(2-methoxyphenoxy) ethylamine on S-carvedilol crystallization purification can be reduced while the S-epoxy carbazole conversion rate is increased, and finally high-yield and high-purity S-carvedilol is prepared.

Description

technical field [0001] The invention relates to a method for continuously producing and separating S-carvedilol by utilizing S-epoxycarbazole and 2-(2-methoxyphenoxy)ethylamine, belonging to the technical field of preparation of S-carvedilol . Background technique [0002] According to WHO estimates, at least 12 million people die from cardiovascular and cerebrovascular diseases in the world every year. Cardiovascular and cerebrovascular diseases have become the number one enemy of human health. Among the top 20 best-selling drugs in the world in 2009, cardiovascular and cerebrovascular disease drugs accounted for 6 of them. It is the largest category of drugs in the world, accounting for about 20% of the total drug market share; in China, cardiovascular and cerebrovascular drugs belong to the second largest category of drugs, accounting for about 15% of the total drug sales in the country. Carvedilol (Daliquan and Coreg) has been showing strong market competitiveness sinc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/88
CPCC07D209/88
Inventor 卢定强俞洋凌岫泉王芳陆步实
Owner JIANGSU SUNAN PHARMA IND CO LTD
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