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Preparation method of unknown impurity of sitagliptin phosphate tablet

A technology of sitagliptin phosphate tablets and sitagliptin impurities, which is applied in the field of preparation of unknown impurities of sitagliptin phosphate tablets, and can solve problems such as increased impurities and poor qualitative and quantitative accuracy

Inactive Publication Date: 2019-12-20
HEFEI HUAFANG PHARMA SCI & TECH +1
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  • Abstract
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  • Claims
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Problems solved by technology

[0010] Neither the European Pharmacopoeia nor the United States Pharmacopoeia contains the impurity Ⅰ in the standards for sitagliptin tablets. During the detection process of related substances in sitagliptin phosphate tablets, an unknown impurity was produced. It may be Ⅰ. There is no reference substance for this impurity on the market, and there is no report on the synthesis method of this impurity in domestic and foreign literature and patents. Currently, the self-control method is used, and its qualitative and quantitative accuracy is not good.

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  • Preparation method of unknown impurity of sitagliptin phosphate tablet
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  • Preparation method of unknown impurity of sitagliptin phosphate tablet

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Embodiment Construction

[0029] In order to make the technical means, creative features, goals and effects achieved by the present invention easy to understand, the present invention will be further elaborated below in conjunction with specific embodiments and illustrations.

[0030] Add 2.00 g of sitagliptin and 0.98 g of maleic anhydride to the reaction flask, add 20 mL of tetrahydrofuran, stir at room temperature until completely dissolved, then add 1.60 g of diazabicyclo, the color of the reaction mixture gradually becomes orange-red, continue stirring at room temperature 3h. After the sitagliptin reaction was complete, 0.70 g of anhydrous potassium carbonate was added into the reaction flask, and 20 mL of water was added at the same time, and stirred at room temperature for 1 h. Then it was extracted twice with 50 mL of dichloromethane, and the organic layer was separated. Slowly add dilute hydrochloric acid to the water layer to adjust the pH to 7, extract twice with 100 mL of dichloromethane, ...

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Abstract

The invention discloses a preparation method of an unknown impurity of a sitagliptin phosphate tablet, and relates to the technical field of organic synthesis. Sitagliptin and maleic anhydride are taken as raw materials to carry out an addition reaction under action of a catalyst to obtain the sitagliptin impurity. The preparation method can be used for efficiently synthesizing the sitagliptin impurity (I), and the structure of the impurity is characterized and determined by nuclear magnetism and mass spectrum; and the impurity is taken as a reference substance to qualitatively and quantitatively analyze whether impurities are generated in a processing or placing process of a siagliptin phosphate preparation and qualitatively and quantitatively analyze the content of the impurities in thesiagliptin phosphate preparation, so that quality control of the siagliptin phosphate preparation can be facilitated and an expected drug effect of the siagliptin phosphate preparation is ensured.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing sitagliptin phosphate tablets with unknown impurities. Background technique: [0002] According to the data and estimates of diabetes and impaired glucose tolerance (IGT) released by the International Diabetes Federation (IDF), the number of diabetic patients in 2003 was 194 million, and it will reach 333 million in 2025; It will be as high as 472 million. In recent years, with the continuous improvement of people's living standards and changes in dietary structure, the number of diabetic patients in my country has also experienced a large-scale increase. [0003] The anti-diabetic drugs currently in clinical use mainly include insulin, sulfonylurea, metformin, and recently listed α-glucosidase inhibitors and insulin sensitizers such as thiazolidinedione drugs. These drugs have a good curative effect, but there are still disadvantages that the ...

Claims

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Application Information

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IPC IPC(8): C07D487/04G01N24/08G01N27/62
CPCC07D487/04G01N24/087G01N27/62
Inventor 孙远东裴小兵杨士伟何勇王锦辉高永好彭扶云任何方宗华于艳英吴宗好
Owner HEFEI HUAFANG PHARMA SCI & TECH
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