Method for separating ranolazine by adopting simulated moving bed

A technology for simulating moving bed and ranolazine is applied in the field of simulated moving bed chromatographic separation of ranolazine, which can solve the problems such as the separation and preparation of ranolazine racemates that have not yet been seen, and achieve continuous automation of production, stable product quality and simple process. Effect

Inactive Publication Date: 2013-03-06
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, some companies in our country have applied for the patent of synthesizing ranolazine, but the synthetic product is a racemate, which is also sold in the market. It has bee...

Method used

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  • Method for separating ranolazine by adopting simulated moving bed
  • Method for separating ranolazine by adopting simulated moving bed

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0030] 1. Preparation of cellulose-tris(3,5-dimethylphenylcarbamate) filler

[0031] Prepare according to the method of literature (Okamoto Y, Kawashima M, Hatada K J . Chromatogr.1986,363:173~186). Cellulose and phenyl isohydrogen were reacted in pyrrole solution at 100°C for 24 hours, and the methanol-incompatible substance obtained from the reaction was cellulose-tris(3,5-dimethylphenylcarbamate). Cellulose-tris(3,5-dimethylphenylcarbamate) was dissolved in tetrahydrofuran, and aminopropyl silica gel was added to the solution, and electromagnetically stirred until the tetrahydrofuran was volatilized, and repeated 3 times to obtain cellulose- Tris(3,5-dimethylphenylcarbamate) coated chiral stationary phase. Wherein the weight ratio of cellulose-three (3,5-dimethylphenylcarbamate) to aminopropyl silica gel is 1:5;

[0032] 2. Selection of mobile phase flow rate

[0033] The flow rate of the mobile phase affects the separation of ranolazine enantiomers and also affects the ...

example 1

[0055] A operating conditions

[0056] Mobile Phase: Methanol

[0057] Injection concentration: 5g / ml

[0058] Injection liquid flow rate: 1.5 ml / min

[0059] Eluent flow rate: 3.0 ml / min

[0060] Extraction flow rate: 2.5 ml / min

[0061] Raffinate flow rate: 2.0 ml / min

[0062] Switching time: 6.8min

[0063] System temperature: 30°C

[0064] B finished product analysis

[0065] Analyzing the composition of the extract and raffinate with an analytical column, the purity of the extract is 99.5%, and the purity of the raffinate is 99.3%. Each kilogram of stationary phase can produce 33.5kg of R-ranolazine and S-ranolazine per day. The phase consumption was 0.128L / kg, and the recovery rate was 99.2%.

[0066]

example 2

[0068] A operating conditions

[0069] Mobile Phase: Methanol

[0070] Injection concentration: 5g / ml

[0071] Injection liquid flow rate: 1.0 ml / min

[0072] Eluent flow rate: 2.5 ml / min

[0073]Extraction flow rate: 1.7 ml / min

[0074] Raffinate flow rate: 1.8 ml / min

[0075] Switching time: 7.5min

[0076] System temperature: 30°C

[0077] B finished product analysis

[0078] Analyzing the composition of the extract and raffinate with an analytical column, the purity of the extract is 99.4%, and the purity of the raffinate is 99.5%. Each kilogram of stationary phase can produce 22kg of R-ranolazine and S-ranolazine per day, and the mobile phase The consumption is 0.163L / kg, and the recovery rate is 97.2%.

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Abstract

The invention discloses a method for separating chiral compound ranolazine by adopting a simulated moving bed in a fourth region. The method is characterized by adopting a simulated moving bed chromatography system, taking cellulose-tris(3,5-dimethylphenylcarbamate) as a filler and methanol as a mobile phase and separating high-purity R-ranolazine and S-ranolazine from racemes of ranolazine. 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 designs a separation technology of chiral drugs, especially a simulated moving bed chromatographic separation method of ranolazine. Background technique [0002] Ranolazine is β-amino alcohol, the chemical name is (±)-N-(2,6-dimethylphenyl)-4-[2-hydroxy-3-(2-methoxyphenoxy)propyl ]-1-piperazineacetamide, English chemical name is (±)-N-(2,6-dimethylphenyl)-4-[2-hydroxy-3-(2-methoxyphenoxy)pmpryl]-1-piperazineacetamide, its molecule The structural formula is: [0003] [0004] Ranolazine is a new type of drug for the treatment of angina-type coronary heart disease developed by CV Therapeutics of the United States. It is called a pFOX (partial fatty acid oxidation) inhibitor. It has no effect on heart rate and blood pressure, can effectively relieve angina, and does not change other drugs Kinetic parameters that improve quality of life in patients with angina. The drug was approved by the U.S. Food and Drug Administration (FDA) in Janu...

Claims

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Application Information

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IPC IPC(8): C07D295/15C07B57/00B01D15/10
Inventor 李枝玲王亚辉李胜迎金新亮王冰冰居延娟罗军侠
Owner JIANGSU HANBON SCI & TECH CO
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