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Method for refining trelagliptin

A refining method, the technology of ethyl acetate, applied in the direction of organic chemistry, can solve the problems of poor cleaning effect, low yield, waste of raw materials, etc., and achieve the effect of improving purity, high yield, and easy operation

Inactive Publication Date: 2017-07-11
合肥拓锐生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There are many refining methods for trexagliptin, but the removal effect on impurity 1, impurity 2, and impurity 3 is not good, and the yield is low, and the waste of raw materials is serious

Method used

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  • Method for refining trelagliptin
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  • Method for refining trelagliptin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A refining method of Trexagliptin, comprising the steps of:

[0036] S1. Mix the crude product of trexagliptin, ethyl acetate and ethanol, reflux and stir for 2-4h, add molecular sieves, continue to reflux and stir for 1-2h, filter while hot to take the filtrate, cool down to 0-5°C, and stir for 2-3h , filter to get the filter cake, and dry to obtain the intermediate;

[0037] S2. Mix the intermediate obtained in S1 with ethyl acetate and isopropanol, reflux and stir for 3-5 hours, cool down to 0-5° C., stir for 3-4 hours, filter to take the filter cake, and dry to obtain Trexagliptin.

Embodiment 2

[0039] A refining method of Trexagliptin, comprising the steps of:

[0040] S1. Mix 1 kg of trexagliptin crude product, 5 L of ethyl acetate and 0.5 L of ethanol, stir at reflux for 3 h, add 0.03 kg of 4A molecular sieve with a particle size of 2 mm, continue stirring at reflux for 1.5 h, filter while hot to take the filtrate, and cool down to 2°C, stirred for 2.5h, filtered to take the filter cake, heated to 57°C, dried under reduced pressure for 10h to obtain 0.927kg of intermediate;

[0041] S2. Mix 0.927 kg of the intermediate obtained in S1 with 4.635 L of ethyl acetate and 1.391 L of isopropanol, stir at reflux for 4 hours, cool down to 3°C, stir for 3.5 hours, filter to take the filter cake, heat up to 57°C, and depressurize After drying for 10 hours, 0.828kg trexagliptin was obtained. The crude product of Trexagliptin and Trexagliptin were detected by high performance liquid chromatography, the results are shown in figure 1 and figure 2 , figure 1 It is the HPLC c...

Embodiment 3

[0043] A refining method of Trexagliptin, comprising the steps of:

[0044] S1. Mix 1 kg of troxagliptin crude product, 9 L of ethyl acetate and 1 L of ethanol, stir at reflux for 2 h, add 0.01 kg of 4A molecular sieves with a particle size of 2.5 mm, continue stirring at reflux for 1 h, filter while hot to take the filtrate, and cool to Stir at 5°C for 2h, filter to take the filter cake, heat up to 60°C, dry under reduced pressure for 8h to obtain 0.905kg of intermediate;

[0045] S2. Mix 0.905 kg of the intermediate obtained in S1 with 5.43 L of ethyl acetate and 1.086 L of isopropanol, stir at reflux for 5 hours, cool down to 0°C, stir for 4 hours, filter to take the filter cake, heat up to 55°C, and dry under reduced pressure 12h obtained 0.802kg trexagliptin.

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Abstract

The invention discloses a method for refining trelagliptin, the method comprises the following steps: S1, evenly mixing crude trelagliptin, ethyl acetate and ethanol, refluxing and stirring for 2-4h, adding a molecular sieve, continuing refluxing and stirring for 1-2h, hotly filtering to obtain filtrate, cooling to 0-5 DEG C, stirring for 2-3h, filtering to obtain a filtering cake, and drying to obtain an intermediate; and S2, evenly mixing the intermediate obtained by the step 1 with ethyl acetate and isopropanol, refluxing and stirring for 3-5h, cooling to 0-5 DEG C, stirring for 3-4h, filtering to obtain a filtering cake, and drying to obtain the trelagliptin. The trelagliptin prepared by the method has the advantages of high purity, good yield, simple operation and low cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical medicine purification, in particular to a method for refining trexagliptin. Background technique [0002] Trelagliptin, the chemical name is 2-({6-[(3R)-3-aminopiperidin-1-yl]-3-methyl-2,4-dioxo-3,4- Dihydropyrimidin-1(2H)-yl}methyl)-4-fluorobenzonitrile, whose molecular formula is C 18 h 20 FN 5 o 2 , the molecular weight is 357.38, the CAS number is 865759-25-7, and its structural formula is as follows: [0003] [0004] Trexagliptin is a dipeptidyl peptidase-4 (DPP-4) inhibitor. By inhibiting the activity of DPP-4, the plasma glucagon-like peptide-1 (GLP-1) activity level continues to increase , GLP-1 is an incretin with glucose-dependent insulin-stimulating properties. It can promote insulin secretion from β cells, inhibit inappropriate glucagon secretion from α cells, delay gastric emptying and suppress appetite. Multiple pathways such as participating in the body's blood sugar home...

Claims

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Application Information

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IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 戴德标陆文通张经伟
Owner 合肥拓锐生物科技有限公司
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