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Method for splitting chlortrimeton enantiomer by using simulated moving bed chromatography

A technique of simulating moving bed and chromatographic separation, which is applied in the field of separation of chiral drugs, can solve problems such as inability to achieve separation effect and low purity, and achieve the effects of continuous automation of production, simple process and stable product quality

Inactive Publication Date: 2015-04-29
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the research on chlorpheniramine enantiomers has mainly focused on the method of constructing a chiral environment and the analysis of purity. Even if the R-chlorpheniramine monomer is separated by traditional chromatographic methods, the purity is low and the ideal separation cannot be achieved. Effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] 1. Sample preparation: The sample is dissolved with a mixed solution of n-hexane and isopropanol (volume ratio 8:1) as the mobile phase to make a concentration of 1g / L, filtered through a 0.45um organic filter membrane for use;

[0026] 2. Determination of simulated moving bed parameters: sample flow rate 6.5mL / min, elution flow rate 65mL / min, extract flow rate 21.6mL / min, raffinate flow rate 15.9mL / min, switching time 6.2min, temperature control at 30 ℃;

[0027] 3. Product collection: After the simulated moving bed system is operating stably, the products are collected from the outlets of the extract and raffinate respectively, and the final products are obtained after concentration under reduced pressure and recrystallization;

[0028] 4. Finished product inspection: After the obtained product is dissolved in the mobile phase, the purity of the collected R-chlorpheniramine and S-chlorpheniramine are detected, which are 99.9% and 99.5% respectively;

[0029] Each kilogram of ...

example 2

[0031] 1. Sample preparation: The sample is dissolved with a mixed solution of n-hexane and isopropanol (volume ratio 9:1) as the mobile phase to make a concentration of 8g / L, filtered through a 0.45um organic filter membrane for use;

[0032] 2. Determination of simulated moving bed parameters: injection flow rate 7.0mL / min, elution flow rate 70mL / min, extract flow rate 23.3mL / min, raffinate flow rate 17.7mL / min, switching time 5.7min, temperature control at 25 ℃;

[0033] 3. Product collection: After the simulated moving bed system is operating stably, the products are collected from the outlets of the extract and raffinate, and the final product is obtained after concentration under reduced pressure and recrystallization;

[0034] 4. Finished product inspection: After the obtained product is dissolved in the mobile phase, the purity of the collected R-Chlorpheniramine and S-Chlorpheniramine are 99.8% and 99.5% respectively;

[0035] Each kilogram of stationary phase can produce 1.9...

example 3

[0037] 1. Sample preparation: the sample is dissolved with a mixed solution of n-hexane and isopropanol (volume ratio 10:1) as the mobile phase to make a concentration of 15g / L, filtered through a 0.45um organic filter membrane for use;

[0038] 2. Determination of simulated moving bed parameters: sample flow rate 7.5mL / min, elution flow rate 75mL / min, extract flow rate 25mL / min, raffinate flow rate 18.4mL / min, switching time 5.3min, temperature control at 35℃ ;

[0039] 3. Product collection: After the simulated moving bed system is operating stably, the products are collected from the outlets of the extract and raffinate respectively, and the final products are obtained after concentration under reduced pressure and recrystallization;

[0040] 4. Finished product inspection: After the obtained product is dissolved in the mobile phase, the purity of the collected R-Chlorpheniramine and S-Chlorpheniramine are determined to be 99.5% and 99.3% respectively;

[0041] Each kilogram of sta...

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PUM

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Abstract

The invention discloses a method for splitting a chlortrimeton enantiomer by using simulated moving bed chromatography. The method is characterized by comprising the following steps: by adopting a simulated moving bed chromatography system, taking silica gel of amylose-tri(3,5-dimethyl phenylcarbamate) as a filler, and taking a mixed solution of normal hexane and isopropyl alcohol as a mobile phase, splitting the chlortrimeton enantiomer under normal phase conditions, thereby obtaining high-purity R-chlortrimeton and S-chlortrimeton. The simulated moving bed chromatography system has the advantages of continuous production, high degree of automation and high production efficiency.

Description

Technical field [0001] The invention relates to a separation technology of chiral drugs, in particular a simulated moving bed chromatography separation method of chlorpheniramine. Background technique [0002] Chlorpheniramine (also known as chlorpheniramine maleate, or chlorpheniramine maleate, or chlorpheniramine maleate), as an excellent antihistamine, has been widely used in daily anti-allergic and anti-cold treatments It is especially suitable for various allergic diseases, including allergic urticaria, facial dermatitis, allergic rhinitis, allergic conjunctivitis, atopic dermatitis, contact dermatitis, insect biting dermatitis, angioedema, allergic Asthma and drug allergy, etc. Chlorpheniramine is a chiral drug. Among them, the pharmacological activity of R-chlorpheniramine is stronger than that of racemate, which is about twice that of the latter, and the side effects are even less common. Therefore, the separation of chiral isomers of chlorpheniramine was carried out. R...

Claims

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Application Information

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IPC IPC(8): C07D213/38
CPCC07D213/38
Inventor 刘玉明王亚辉严忠居延娟李枝玲张大兵
Owner JIANGSU HANBON SCI & TECH CO
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