Omarigliptin refining method

A refining method and prescription technology, which are applied in the fields of pill delivery, metabolic diseases, organic chemistry, etc., can solve the problems of difficulty in refining work, low solubility, poor solubility of augliptin, etc., and achieve the effect of easy operation and simple method.

Inactive Publication Date: 2018-03-23
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Alogliptin has poor solubility, it is insoluble in water, and its solubility in alcohol solvents is also very low, which brings certain difficulties to the refining work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The first step dissolves 17g augliptin crude product in 100ml hexamethylphosphoramide;

[0027] Step 2: At room temperature, add 1.36 g of activated carbon to the solution in Step 1, stir for 1.2 hours, and filter;

[0028] In the third step, under stirring, the temperature of the filtrate in the second step is lowered to -10°C, and 40ml of the mixed solution of hexamethylphosphoramide-acetone is slowly added dropwise to it, and the speed of adding the mixed solution of hexamethylphosphoramide-acetone is 2.5ml / min; a white solid was precipitated, and the stirring was continued for 5 hours, and the stirring speed was at 200 rpm; in the mixed solvent, the volume ratio of hexamethylphosphoramide-acetone was 5:2.

[0029] The fourth step is to filter, and the filter cake is beaten with 100ml of isopropanol, and stirred for 1 hour;

[0030] The fifth step is to filter, and the filter cake is washed 3 times with isopropanol, and the dosage is 8ml each time.

[0031] Step 6...

Embodiment 2

[0034] The first step 26g alogliptin crude product is dissolved in 100ml hexamethylphosphoramide;

[0035] Step 2 At room temperature, add 2.6 g of activated carbon from the first step to the solution in the first step, stir for 2 hours, and filter;

[0036] Step 3 Under stirring, cool down the filtrate of the second step to 0°C, slowly add 65ml of hexamethylphosphoramide-acetone mixed solution dropwise, and a white solid precipitates out; continue stirring for 5-8 hours;

[0037] The speed of adding hexamethylphosphoramide-acetone mixed solution dropwise in this step is 4.5ml / min, and in the mixed solvent, the volume ratio of hexamethylphosphoramide-acetone is 5:2.8; minute

[0038] The fourth step is to filter, and the filter cake is beaten with 100ml of isopropanol, and stirred for 1 hour;

[0039] The fifth step is to filter, and the filter cake is washed 3 times with isopropanol, and the dosage is 8ml each time.

[0040] Step 6 Spread the filter cake and dry it under v...

Embodiment 3

[0043] The first step 20g alogliptin crude product is dissolved in 100ml hexamethylphosphoramide;

[0044] Step 2: At room temperature, add 1.9 g of activated carbon to the solution in Step 1, stir for 1.52 hours, and filter;

[0045] Under stirring in the third step, the temperature of the filtrate in the second step was lowered to -50°C, and 58ml of a mixed solution of hexamethylphosphoramide-acetone was slowly added dropwise to it, and a white solid was precipitated, and the stirring was continued for 5-8 hours; the mixed solvent Among them, the volume ratio of hexamethylphosphoramide-acetone is 5:2.5; the speed of dropping the mixed solution of hexamethylphosphoramide-acetone is 3.6ml / min; the speed of continuous stirring is 245 rpm.

[0046] The fourth step is to filter, and the filter cake is beaten with 100ml of isopropanol, and stirred for 1 hour;

[0047] The fifth step is to filter, and the filter cake is washed 3 times with isopropanol, and the dosage is 8ml each t...

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PUM

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Abstract

The invention relates to a method for refining alogliptin, which belongs to the technical field of preparation of raw materials. The technical scheme of the present invention is: dissolve the crude product of alogliptin in hexamethylphosphoramide; add a certain amount of activated carbon, stir, and filter; The mixed solution of base phosphoramide-acetone, white solid is separated out, continue stirring for 5-8 hours; Filter, filter cake is beaten with isopropanol of the same volume as the first step, stir for 1 hour; Filter, filter cake is with isopropanol After washing, the filter cake was spread out and dried under vacuum at 25°C. The invention provides a method for refining alogliptin. The method of the invention is simple, easy to operate and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for refining alogliptin, which belongs to the technical field of raw material medicine preparation. Background technique [0002] Diabetes is a group of metabolic diseases characterized by hyperglycemia. Hyperglycemia is caused by defective insulin secretion or impaired biological action, or both. The long-term high blood sugar in diabetes leads to chronic damage and dysfunction of various tissues, especially the eyes, kidneys, heart, blood vessels, and nerves. It seriously affects the quality of life of patients. [0003] The International Diabetes Federation estimates that by 2035 there will be 592 million people with diabetes worldwide. About 80% of people with diabetes live in low- and middle-income countries. In China, the prevalence of diabetes is increasing rapidly. National Diabetes Survey Comparison Between 1981 and 2010, the prevalence of diabetes in my country increased by 17 times. [0004] According ...

Claims

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Application Information

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IPC IPC(8): C07D487/04A61K31/4162A61K9/20A61P3/10
CPCC07D487/04A61K9/2059A61K31/4162
Inventor 孙爱梅
Owner WEIHAI GUANBIAO INFORMATION TECH
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