Method for reducing palladium residue in compound and preparation method of high-purity fosaprepitant dimeglumine by applying method

A technology for compound and palladium residue, applied in the field of medicine, can solve problems such as limited application and difficult operation, and achieve the effect of simplifying experimental operation and high purity

Active Publication Date: 2012-12-26
JIANGSU AOSAIKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 100g of aprepitant monobenzyl phosphate and 55.4g of N-methyl-D-glucosamine into the hydrogenation kettle, add 10g of 10% palladium on carbon, add 800ml of methanol and 50ml of water, at room temperature, at 0.45MPa After pressure hydrogenation for 12 hours, the reaction solution was filtered with a 0.22-micron microporous membrane, and the obtained filtrate was a slightly yellow clear solution. 10 μg of triphenylphosphine and 10 μl of tributylphosphine were added to the reaction solution. Under gas protection, stir at room temperature for 12 hours. Then the reaction solution was concentrated under reduced pressure in a water bath at 30 degrees Celsius to about 200ml, passed through a constant pressure dropping funnel, and added dropwise to 2L of acetonitrile with stirring, a white solid was precipitated, filtered under nitrogen protection, and the obtained solid was filtered under vacuum. After drying at room temperature, 102 g of fosaprepitant dimeglumine was obta...

Embodiment 2

[0046]Add 100g of aprepitant monobenzyl phosphate and 55.4g of N-methyl-D-glucosamine into the hydrogenation kettle, add 10g of 10% palladium on carbon, add 800ml of methanol and 50ml of water, at room temperature, at 0.45MPa After pressure hydrogenation for 12 hours, the reaction solution was filtered with a 0.22-micron microporous membrane, and the obtained filtrate was a slightly yellow clear solution. 10 μg of triphenylphosphine and 10 μl of tributylphosphine were added to the reaction solution. Under air protection, stir at room temperature for 8 hours. Then the reaction solution was concentrated under reduced pressure in a water bath at 30 degrees Celsius to about 200ml, passed through a constant pressure dropping funnel, and added dropwise to 2L of acetonitrile with stirring, a white solid was precipitated, filtered under nitrogen protection, and the obtained solid was filtered under vacuum. After drying at room temperature, 99 g of fosaprepitant dimeglumine was obtaine...

Embodiment 3

[0049] Add 100g of aprepitant monobenzyl phosphate and 55.4g of N-methyl-D-glucosamine into the hydrogenation kettle, add 10g of 10% palladium on carbon, add 800ml of methanol and 50ml of water, at room temperature, at 0.45MPa After pressure hydrogenation for 12 hours, the reaction solution was filtered with a 0.22-micron microporous membrane, and the obtained filtrate was a slightly yellow clear solution. 10 μg of triphenylphosphine and 10 μl of tributylphosphine were added to the reaction solution. Under air protection, stir at room temperature for 18 hours. Then the reaction solution was concentrated under reduced pressure in a water bath at 30 degrees Celsius to about 200ml, passed through a constant pressure dropping funnel, and added dropwise to 2L of acetonitrile with stirring, a white solid was precipitated, filtered under nitrogen protection, and the obtained solid was filtered under vacuum. After drying at room temperature, 97 g of fosaprepitant dimeglumine was obtai...

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Abstract

The invention belongs to the field of medicines, and relate to a method for reducing palladium residue in a compound and a preparation method of high-purity fosaprepitant dimeglumine by applying the method. In the method, tributyl phosphane and triphenyl phosphine are used as palladium removing agent to treat compound solution. After palladium is removed by using the method, the high-purity fosaprepitant dimeglumine can be obtained through crystallization with poor solvent in one step. The residue of tributyl phosphane and triphenyl phosphine in a finished product is low, and the palladium residue limit is less than 1 ppm, therefore, the requirement of limit of palladium residue in crude drug for injection is satisfied, and the industrial production after magnification is further adapted.

Description

[0001] technical field [0002] The invention belongs to the field of medicine, and relates to a method for reducing palladium residues in compounds, in particular to a method for preparing high-purity fosaprepitant dimeglumine using the method. [0003] Background technique [0004] In the field of medicine preparation, especially in the preparation method of fosaprepitant dimeglumine, the catalysis of palladium-carbon is often involved, so it is necessary to add palladium-carbon in the reaction process, but after the reaction is over, a certain amount of time must be passed. method to control the residual amount of palladium. Therefore, whether palladium residues can be controlled below the limit required by regulations, and whether other substances are produced during the palladium removal process, especially whether other harmful substances are introduced, have become the research focus of this type of preparation method. [0005] Aprepitant is an adjuvant drug used du...

Claims

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Application Information

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IPC IPC(8): C07F9/6558
Inventor 赵小伟宗在伟刘子宁
Owner JIANGSU AOSAIKANG PHARMA CO LTD
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