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Method for resolving pantolactone enantiomers by adopting simulated moving bed chromatography

A technology for simulating moving bed and separating pantolactone, which is applied in the field of chiral compound separation to achieve the effects of less eluent, good separation ability and high separation purity

Active Publication Date: 2021-03-05
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Simulated moving bed chromatography is an efficient separation technology developed in recent years. It is a combination of simulated moving bed technology and chromatography. Its principle is similar to that of single column chromatography. It is based on the adsorption and separation of different components in the stationary phase and mobile phase. Separation is achieved with different distribution coefficients. The difference is its mode of operation, which can achieve continuous operation without the need to use expensive resolving agents, and can avoid environmental pollution and toxicity problems. However, this technology is applied to the actual resolution of specific enantiomers At the same time, it is also necessary to consider the separation ability of the technology for two specific enantiomers (including product yield, purity, and processing capacity per unit time, etc.). Only with better separation ability can it be suitable for large-scale continuous separation. It has the advantages of high separation efficiency, saving packing, and low cost, so it has the value of replacing other separation methods. At present, there is no report on the application of simulated moving bed chromatography technology to the separation of D,L-panthenolactone

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  • Method for resolving pantolactone enantiomers by adopting simulated moving bed chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 (φ10mm*100mm*4)

[0045] 1. Sample preparation: the sample was dissolved with eluent (60 ethanol: 40 ethyl acetate, v: v) to make a concentration of 40 mg / mL, and filtered through a 0.45 μm organic filter membrane for later use;

[0046]2. Selection of simulated moving bed parameters: Determine the parameters as follows: injection flow rate 1mL / min, elution flow rate 10mL / min, extract flow rate 6mL / min, raffinate flow rate 5mL / min, switching time 15min, temperature control at 20 ~30°C;

[0047] 3. Product collection: After the simulated moving bed system is running stably, the products are collected from the two outlets respectively, concentrated under reduced pressure, and crystallized to obtain the final product;

[0048] 4. Finished product inspection: After the obtained product is dissolved in mobile phase, the purity of the two export products D-pantothenolactone and L-pantothenolactone are detected by analytical conditions to be 99.6% and 98.0% respecti...

Embodiment 2

[0050] Example 2 (φ10mm*100mm*8)

[0051] 1. Sample preparation: the sample was dissolved with eluent (70 ethanol: 30 ethyl acetate, v: v) to make a concentration of 80 mg / mL, and filtered through a 0.45 μm organic filter membrane for later use;

[0052] 2. Selection of simulated moving bed parameters: Determine the parameters as follows: injection flow rate 3mL / min, elution flow rate 20mL / min, extract flow rate 12mL / min, raffinate flow rate 11mL / min, switching time 14min, temperature control at 20 ~30°C;

[0053] 3. Product collection: After the simulated moving bed system is running stably, the products are collected from the two outlets respectively, concentrated under reduced pressure, and crystallized to obtain the final product;

[0054] 4. Finished product inspection: After the obtained product is dissolved in mobile phase, the purity of the two exported products D-pantothenolactone and L-pantothenolactone are detected by analytical conditions to be 99.4% and 97.6% res...

Embodiment 3

[0056] Example 3 (φ15mm*100mm*8)

[0057] 1. Sample preparation: Dissolve the sample with an eluent (80 ethanol:20 ethyl acetate, v:v) to make a concentration of 200 mg / mL, and filter it through a 0.45 μm organic filter membrane for later use;

[0058] 2. Selection of simulated moving bed parameters: Determine the parameters as follows: injection flow rate 6mL / min, elution flow rate 33mL / min, extract flow rate 20mL / min, raffinate flow rate 19mL / min, switching time 12min, temperature control at 20 ~30°C;

[0059] 3. Product collection: After the simulated moving bed system is running stably, the products are collected from the two outlets respectively, concentrated under reduced pressure, and crystallized to obtain the final product;

[0060] Finished product inspection: After the obtained product is dissolved in mobile phase, the purity of the two exported products D-pantothenolactone and L-pantothenolactone are detected by analytical conditions to be 99.2% and 95.3% respecti...

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Abstract

The invention discloses a method for resolving pantolactone enantiomers by adopting simulated moving bed chromatography, which comprises the following steps: injecting a pantolactone sample solution to be separated into a feeding point of the simulated moving bed chromatography, injecting eluent into an eluent input point of the simulated moving bed chromatography, and respectively collecting twoenantiomers of pantolactone from an extraction point and a raffinate point of simulated moving bed chromatography. The method is low in cost, good in separation efficiency, capable of achieving continuous production and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of separation of chiral compounds, and in particular relates to a method for separating pantothenolactone enantiomers by using simulated moving bed chromatography. Background technique [0002] Panthenolactone, also known as dihydro-3-hydroxy-4,4-dimethyl-2(3H)-furanone, is an important pharmaceutical intermediate, which can be used to synthesize calcium pantothenate (also known as vitamin B5 ) and panthenol (also known as provitamin B5), see Schnider, O.: Synthesis of panthenol and its transformation into pantothenic acid. Jubilee Vol. EmilBarell 1946, 85-91 and other reports. [0003] Panthenolactone is divided into 3 forms: mixed body (DL-type), right-handed body (D-type) and left-handed body (L-type), among which D-panthenolactone is the most useful, because D-panthenyl Lactones can selectively synthesize calcium D-pantothenate and D-panthenol. [0004] D-panthenolactone is generally obtained by splitt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01D15/18B01D15/42
CPCC07D307/33B01D15/185B01D15/426C07B2200/07
Inventor 李博康宁王钰涂仕春张伟王玉岗林波俞宏伟郑思敏
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD