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Ticagrelor chiral intermediate liquid chromatographic analysis method

A technique for liquid chromatography analysis, chiral intermediates

Active Publication Date: 2018-05-15
ZHEJIANG TIANYU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The ultraviolet absorption of the above-mentioned ticagrelor chiral intermediate and its enantiomers is relatively weak, and the conventional high-performance liquid chromatography (HPLC) with an ultraviolet detector cannot detect this chiral intermediate and its opposite sensitively. The content of enantiomers, there is a problem that the sample is not easy to be detected

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Experimental program
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Embodiment Construction

[0036] specific implementation plan

[0037] Testing equipment : High performance liquid chromatography equipped with UV detector

[0038] Chromatographic conditions :

[0039] Chromatographic column: Agilent ZORBAX XDB-C8 4.6×250mm, 5um

[0040] Mobile phase: Mobile phase A: Accurately weigh 1.36g KH 2 PO 4 Dissolve in 1000mL ultrapure water with 20% H 3 PO 4 Adjust the pH of the solution to 3.0; mobile phase B: acetonitrile

[0041] Detection wavelength: 340nm

[0042] Flow rate: 1.0mL / min

[0043] Column temperature: 35°C

[0044] Injection volume: 20μL

[0045] Running time: 55min

[0046] Mobile phase gradient:

[0047]

[0048] Solution preparation :

[0049] Diluent: mobile phase A-acetonitrile (70:30 (v / v)).

[0050] Need test solution: Accurately weigh 40mg ticagrelor chiral intermediate sample (2-[[(3aR,4S,6R,6aS)-6-aminotetrahydro-2,2-dimethyl-4H-cyclo Pentene-1,3-dioxolan-4-yl]oxyl]ethanol) was dissolved in a 10mL volumetric flask with ultrap...

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Abstract

The invention provides a ticagrelor chiral intermediate liquid chromatographic analysis method. A chiral intermediate is 2-[(3aR,4S,6R,6aS)-6-amino tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3- dioxolane-4-yl] oxy] ethanol. The method comprises the following steps: respectively and accurately weighing a ticagrelor chiral intermediate solution, a sodium bicarbonate aqueous solution, and a derivative reagent solution, performing vortex mixing, performing a reaction for a certain time, adding a hydrogen chloride aqueous solution, and performing vortex mixing to obtain a ticagrelor chiral intermediate derivative solution; and performing chromatographic analysis on the ticagrelor chiral intermediate derivative solution. The liquid chromatographic analysis method can accurately and sensitively detect the content of the chiral intermediate and its enantiomer.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a liquid chromatography analysis method for a chiral intermediate of ticagrelor. Background technique [0002] 2-[[(3aR,4S,6R,6aS)-6-aminotetrahydro-2,2-dimethyl-4H-cyclopentene-1,3-dioxolan-4-yl]oxy Base] ethanol is an important chiral intermediate in the synthesis of ticagrelor, and its enantiomer 2-[[(3aS,4R,6S,6aR)-6-aminotetrahydro-2,2-di Methyl-4H-cyclopentene-1,3-dioxolan-4-yl]oxyl]ethanol usually exists in the commercially available ticagrelor chiral intermediate products, and the structural formulas of the two are respectively as follows: [0003] [0004] The ultraviolet absorption of the above-mentioned ticagrelor chiral intermediate and its enantiomers is relatively weak, and the conventional high-performance liquid chromatography (HPLC) with an ultraviolet detector cannot detect this chiral intermediate and its opposite sensitively. The content of enantiomers has the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74G01N30/06C07D317/44
CPCC07D317/44G01N30/02G01N30/06G01N30/74G01N2030/067
Inventor 夏仁涨詹六月应燕飞李美君屠勇军
Owner ZHEJIANG TIANYU PHARMA
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