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Method for preparing impurity C reference substance of Trelagliptin succinate

The technology of a trelagliptin succinate and a reference substance is applied in the field of preparation of an impurity C reference substance of trilagliptin succinate, and can solve the problems of low yield, difficult purification and the like

Inactive Publication Date: 2016-09-21
WEIHAI DISU PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN 105524044 A discloses the preparation method of impurity C, which is a multi-step synthesis with low yield and difficult purification (purification by column chromatography)

Method used

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  • Method for preparing impurity C reference substance of Trelagliptin succinate

Examples

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Embodiment 1

[0016] Example 1 Preparation of Trexagliptin Succinate Impurity C Crude Product

[0017] Add 475g (1mol) of trexagliptin succinate and drinking water (3000mL) into the reaction kettle, and stir to dissolve. The temperature was raised to reflux for 36 hours. HPLC monitoring showed that 0.1% of trexagliptin succinate remained, and the reaction was stopped. Concentrated under reduced pressure to obtain the crude product of trexagliptin succinate impurity C (off-white solid), with a content of 95.2% as determined by HPLC. The yield is 100%.

Embodiment 2

[0018] Example 2 Preparation of Trexagliptin Succinate Impurity C Reference Substance

[0019] Add 47.5g (0.1mol) of the product of Example 1 and ethanol (500ml) into a 1000ml three-necked flask, heat up and reflux to dissolve, stir to cool down to 10-25°C, stir for 2h, filter, and dry to obtain the impurity of Trexagliptin succinate C reference substance 42.8g, yield 90%, HPLC assay content 99.4%.

Embodiment 3

[0020] Example 3 Preparation of Trexagliptin Succinate Impurity C Reference Substance

[0021] Add 47.5g (0.1mol) of the product of Example 1 and methanol (300ml) to a 1000ml three-necked flask, heat up and reflux to dissolve, stir to cool down to 10-25°C, stir for 2h, filter, and dry to obtain the impurity of trelagliptin succinate C reference substance 40g, yield 84%, HPLC assay content 98.9%.

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Abstract

The invention relates to a method for preparing an impurity C reference substance of Trelagliptin succinate. The technical scheme of the invention is as follows: the method comprises the steps: (1) carrying out refluxing on Trelagliptin succinate, which serves as a raw material, and a protonic solvent which serves as a solvent, so as to prepare an impurity C of the Trelagliptin succinate; (2) refining a crude product, thereby obtaining the qualified impurity C reference substance. The method for preparing the impurity C reference substance of the Trelagliptin succinate, provided by the invention, is easy and feasible and is used for providing the satisfactory impurity C reference substance for quality control on the Trelagliptin succinate.

Description

technical field [0001] The invention relates to a preparation method of a reference substance of troxagliptin succinate impurity C, belonging to the technical field of chemical synthesis. Background technique [0002] Trelagliptin succinate (Formula I) is a once-weekly dipeptidyl peptidase IV (DPP-4) inhibitor that controls blood glucose levels through selective and sustained inhibition of DPP-4. DPP-4 is an enzyme that triggers the inactivation of incretins (glucagon-like peptide-1 (GLP-1) and glucose-dependent insulinotropic polypeptide (GIP), which are It plays an important role in regulation.Inhibition of DPP-4 can increase blood glucose level-dependent insulin secretion, thereby controlling blood glucose levels. [0003] Trexagliptin succinate was listed in Japan on March 26, 2015 by Takeda Corporation of Japan. According to data query and experimental comparison, it was found that the content of a certain impurity in the raw material drug of the original product was ...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 丛日刚刘江夏克波刘春姜晓军王海波李西贺
Owner WEIHAI DISU PHARMA CO LTD
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