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A method for HPLC analysis and preparation of n-(p-toluenesulfonyl)-l-alanine and its enantiomers

A technology of p-toluenesulfonyl and enantiomers, which is applied in the field of chemical raw material preparation, can solve problems such as no related reports on the method, and achieve the effects of quality assurance, good separation effect, accurate and efficient analysis and separation

Active Publication Date: 2021-03-12
吉林百纯化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In recent years, with the diversification of chiral chromatographic fillers, the application of chiral chromatographic column liquid chromatography has become more and more extensive. However, the analysis and preparation of N-(p-toluenesulfonyl)-L-alanine and its para- There is no relevant report on the method of enantiomer

Method used

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  • A method for HPLC analysis and preparation of n-(p-toluenesulfonyl)-l-alanine and its enantiomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Analysis and separation of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine

[0032] Instruments and Conditions

[0033] Column: IA-H (250×4.6mm, 5.0μm)

[0034] Mobile phase: n-hexane-isopropanol-trifluoroacetic acid aqueous solution (70:30:0.15)

[0035] Column temperature: 40°C

[0036] Flow rate: 0.8mL / min

[0037] Injection volume: 5μL

[0038] Sample concentration: 1mg / mL

[0039] Detection wavelength: 220nm

[0040] Experimental procedure

[0041] Accurately measure 1 mg each of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, Shake well as a reference solution. Accurately weigh 10 mg of N-(p-toluenesulfonyl)-DL-alanine, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 5 μL each of the reference...

Embodiment 2

[0043] Embodiment 2: Analysis and separation of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine

[0044] Instruments and Conditions

[0045] Column: IA-H (250×4.6mm, 5.0μm)

[0046] Mobile phase: n-heptane-ethanol-trifluoroacetic acid (50:50:0.05)

[0047] Column temperature: 20°C

[0048] Flow rate: 0.4mL / min

[0049] Injection volume: 10μL

[0050] Sample concentration: 0.1mg / mL

[0051] Detection wavelength: 220nm

[0052] Experimental procedure

[0053] Accurately measure 1 mg each of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, Shake well as a reference solution. Accurately weigh 10 mg of N-(p-toluenesulfonyl)-DL-alanine, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 1mL of the mother solution of the test produc...

Embodiment 3

[0055] Embodiment 3: Analysis and separation of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine

[0056] Instruments and Conditions

[0057] Column: IA-H (250×4.6mm, 5.0μm)

[0058] Mobile phase: cyclohexane-ethanol-trifluoroacetic acid (60:40:0.16)

[0059] Column temperature: 30°C

[0060] Flow rate: 0.8mL / min

[0061] Injection volume: 5μL

[0062] Sample concentration: 1mg / mL

[0063] Detection wavelength: 220nm

[0064] Experimental procedure

[0065] Accurately measure 1 mg each of N-(p-toluenesulfonyl)-L-alanine and N-(p-toluenesulfonyl)-D-alanine respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, Shake well as a reference solution. Accurately weigh 10 mg of N-(p-toluenesulfonyl)-DL-alanine, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 5 μL each of the reference substance and the...

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Abstract

The invention discloses a method for analyzing and preparing N-(p-toluenesulfonyl)-L-alanine and its enantiomers by HPLC. The polysaccharide derivative is used as the chiral stationary phase, and the non-polar-L-alanine is used as the The polar mixed solvent was used as mobile phase, and normal phase chromatography was used for analysis and separation. The method can analyze and prepare a single optically active N-(p-toluenesulfonyl)-L-alanine and its enantiomer simply, accurately and efficiently, so as to realize its quality control.

Description

technical field [0001] The invention relates to a chromatographic analysis and separation method, especially a high-performance liquid chromatography method for analyzing and preparing N-(p-toluenesulfonyl)-L-alanine and its enantiomers, which belongs to the preparation of chemical raw materials technology field. [0002] technical background [0003] Pyrrolyl ester (chemical name: 3-(N-p-toluenesulfonyl-L-alanyloxy)-5-phenylpyrrole and indole ester (chemical name 3-(N-p-toluenesulfonyl-L-propane Aminoacyloxy)-indole) is a common substrate used in the determination of leukocyte diagnostic reagents, and N-(p-toluenesulfonyl)-L-alanine is the key chiral intermediate in the synthesis process of the substrate, Therefore, how to analyze and prepare N-(p-toluenesulfonyl)-L-alanine and its enantiomers, and then control the quality of N-(p-toluenesulfonyl)-L-alanine is particularly important The structures of N-(p-toluenesulfonyl)-L-alanine and its enantiomers are shown in formula ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 修志明王淑红王丽萍刘莉
Owner 吉林百纯化学科技有限公司
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