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Preparation method of sitagliptin intermediate

A compound, selected technology, applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., can solve problems such as the environment and adverse effects of operators

Active Publication Date: 2014-07-09
SUNSHINE LAKE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] A kind of method for preparing sitagliptin intermediate is provided here, by using low toxicity reaction solvent, solves the problem of the bad influence of existing method to environment and operator, is suitable for industrialized large-scale production; And can high yield This intermediate was prepared in high purity

Method used

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  • Preparation method of sitagliptin intermediate
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  • Preparation method of sitagliptin intermediate

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specific Embodiment approach

[0032] In order to enable those skilled in the art to better understand the technical solutions of the present invention, some non-limiting examples are further disclosed below to further describe the present invention in detail.

[0033] The reagents used in the present invention can be purchased from the market or can be prepared by the methods described in the present invention.

Embodiment 1

[0035] 17.85 grams of monoethyl malonate potassium salt, 22 milliliters of triethylamine and 11.97 grams of anhydrous magnesium chloride were added to 120 milliliters of stirred anhydrous ethyl acetate, and stirred at room temperature for 2 hours; 2,4,5-trifluoro Stir 9.5 g of phenylacetic acid and 9.73 g of N,N'-carbonyldiimidazole in 50 ml of ethyl acetate for 0.5 hours, then add the mixture to the aforementioned reaction solution; the mixed reaction solution is stirred at 50°C-60°C for reaction After 6 hours to 8 hours, lower the temperature to 15°C-25°C, add 10% hydrochloric acid aqueous solution, adjust the pH to less than 3, separate layers, wash the organic layer with saturated brine three times, dry the organic layer with anhydrous sodium sulfate and concentrate Evaporate to dryness to obtain 13.2 g of oil.

Embodiment 2

[0037] 17.85 grams of monoethyl malonate potassium salt, 22 milliliters of triethylamine and 11.97 grams of anhydrous magnesium chloride were added to 120 milliliters of stirred isopropyl acetate, stirred at room temperature for 2 hours, and 2,4,5-trifluorobenzene Stir 9.5 g of acetic acid and 9.73 g of N,N'-carbonyldiimidazole in 50 ml of isopropyl acetate for 0.5 hour, add this mixture to the aforementioned reaction solution, and stir the mixed reaction solution at 50°C-60°C for reaction After 6 hours to 8 hours, lower the temperature to 15°C-25°C, add 10% hydrochloric acid aqueous solution, adjust the pH to less than 3, separate layers, wash the organic layer with saturated brine three times, dry the organic layer with anhydrous sodium sulfate and concentrate Evaporate to dryness to obtain 13.1 g of oil.

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Abstract

The invention relates to a preparation method of a sitagliptin intermediate. The method utilizes a low-toxicity organic solvent as a reaction solvent, realizes high-yield preparation of a high-purity desired product, is conducive to safe production and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a medicine and an intermediate thereof, and belongs to the technical field of pharmacy. Background technique [0002] Sitagliptin, an oral antihyperglycemic drug, improves glycemic control in patients with type 2 diabetes by increasing the levels of active incretin hormones. [0003] In the method for preparing sitagliptin, need to prepare a kind of important intermediate earlier, its structure is as shown in (I1), [0004] [0005] The safe and efficient large-scale industrial production of intermediate (I1) is of great significance to the industrial production of sitagliptin; in the methods for preparing sitagliptin in many documents, acetonitrile, tetrahydrofuran, etc. are used as reaction solvents for the preparation of this intermediate . [0006] In the preparation process, the solvents used have different toxicities to the health of workers and different effects on the quality of drugs accord...

Claims

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Application Information

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IPC IPC(8): C07C69/738C07C67/343
CPCC07C67/343C07C69/738
Inventor 赖金强梁志广杨凤智
Owner SUNSHINE LAKE PHARM CO LTD
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