Method for refining trelagliptin succinate

A technology of trelagliptin succinate and a purification method, applied in the field of pharmacy, can solve the problems of low purity of trelagliptin succinate, being difficult to be applied in industrial production, difficult to remove residual solvent, etc., achieving easy control of solvent residue, The effect of producing green environmental protection and improving drug safety

Active Publication Date: 2016-11-16
NANJING VARSAL MEDICINE TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The limitations of this method are: the purity of the products made from these toxic solvents is low, and the residual solvents in the products are difficult to remove. In addition, these solvents are difficult to be used in industrial production due to their high toxicity or spontaneous combustion.
Although this method avoids the use of dimethylformamide, trifluoroethanol, toluene, 1,4-dioxane, diethyl ether and other solvents that are not conducive to product quality, the impurities that may be produced in the salt-forming process As well as the incompletely salified trexagliptin or succinic acid, it is difficult to obtain high-quality qualified products through refining, which brings hidden dangers to the quality of the product, resulting in low purity of succinate trexagliptin or unqualified succinic acid content, And the yield is low

Method used

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  • Method for refining trelagliptin succinate
  • Method for refining trelagliptin succinate
  • Method for refining trelagliptin succinate

Examples

Experimental program
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Embodiment 1

[0039] The refining method of the trexagliptin succinate provided by the present embodiment comprises:

[0040] Heat 800mL of a mixed solution of water and methanol mixed at a volume ratio of 1:5 to 50°C, then mix with 100g of trexagliptin succinate, and stir until clear to obtain a trexagliptin succinate solution.

[0041] Then, the temperature of the succinate trexagliptin solution was lowered to 2°C, and after crystallization, it was filtered, and the filter cake was washed with methanol and dried to obtain a white solid, that is, refined succinate trexagliptin.

Embodiment 2

[0043] The refining method of the trexagliptin succinate provided by the present embodiment comprises:

[0044] First, prepare 1000 mL of a mixed solution of water and acetone at a volume ratio of 1:9, then add 100 g of trexagliptin succinate to the mixed solution, heat to 55°C and stir until clear to obtain a trexagliptin succinate solution.

[0045] Then place the succinate trexagliptin solution in a fume hood, stir and crystallize for 60 minutes, filter, and wash the filter cake with acetone, then dry it under normal pressure at 50°C for 10 hours to obtain a white solid, that is, refined amber Trexagliptin.

Embodiment 3

[0047] The refining method of the trexagliptin succinate provided by the present embodiment comprises:

[0048] Heat 1000mL of a mixed solution of water and ethanol at a volume ratio of 1:10 to 60°C, then mix it with 100g of trexagliptin succinate, and stir until clear to obtain a trexagliptin succinate solution.

[0049] Then reduce the temperature of the succinate solution to 2°C, crystallize for 60 minutes, filter, and wash the filter cake with ethanol, and then dry it under normal pressure at 55°C for 8 hours to obtain a white solid, that is, refined amber Trexagliptin.

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Abstract

The invention provides a method for refining trelagliptin succinate, wherein the method includes a dissolution step and a crystallization and separation step; the dissolution step comprises the steps of under a condition of the temperature of 30-70 DEG C, mixing a trelagliptin succinate crude product, water and an organic solvent to make the trelagliptin succinate crude product dissolved; the volume ratio of water to the organic solvent is 1 to (5-15), and the organic solvent is selected from at least one of methanol, propanol, acetone, ethanol and isopropanol. The method is used for recrystallization of the trelagliptin succinate crude product, the experimental period is short, the purification yield can be improved, and impurities also can be effectively removed; the obtained trelagliptin succinate has high purity, the purity is more than 99.9% through HPLC detection, and the product quality and the drug use safety are improved significantly.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a method for refining trexagliptin succinate. Background technique [0002] Trelagliptin (Trelagliptin, referred to as Tre) is a dipeptidyl peptidase IV (DPP-4) inhibitor, its structural formula is as follows, [0003] [0004] Clinically use its succinate, ie trexagliptin succinate. Trexagliptin succinate controls blood sugar levels by selectively and persistently inhibiting DPP-4. DPP-4 is an enzyme that triggers the inactivation of incretins and glucose-dependent insulinotropic polypeptides, two incretins that play an important role in blood glucose regulation. Inhibition of DPP-4 can increase blood sugar level-dependent insulin secretion, thereby controlling blood sugar levels. [0005] At present, in the refining method of trexagliptin succinate reported in patents and literatures, dimethylformamide, 1,4-dioxane, ether, trifluoroethanol, toluene and other toxic substances are u...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07B2200/13C07D401/04
Inventor 扈田进张德伟孙珏
Owner NANJING VARSAL MEDICINE TECH DEV
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