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Purification method of indometacin

A technology of indomethacin and purification method, applied in the direction of organic chemistry, etc., can solve problems such as product impurities exceeding the standard

Inactive Publication Date: 2020-10-30
河南优凯制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The introduction of indomethacin methyl ester or indomethacin ethyl ester into the finished product of indomethacin will cause the product impurities to exceed the standard, so it is urgent to find a new crystallization method for the purification of indomethacin

Method used

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  • Purification method of indometacin
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Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 20g of indomethacin crude product and 160g of acetone / water mixed solvent (the volume ratio of acetone to water is 2:1) into a 500ml three-neck flask, stir and heat up to dissolve completely, add 1g of activated carbon, continue to heat up to reflux, and stir for 1h to decolorize ; Filtrate while hot, remove activated carbon, obtain filtrate, filtrate is slowly cooled to 0 ~ 5 ° C, heat preservation and crystallization for 2 ~ 3 hours, filter to obtain crystals, crystals are vacuum dried at 50 ° C for 4 hours, and 18.4 g of pure indomethacin is obtained, with a yield of 92% , 100.0% purity.

[0034] Implementation 2

[0035] Add 20g of indomethacin crude product and 140g of tetrahydrofuran / water mixed solvent (the volume ratio of tetrahydrofuran to water is 3:1) into a 500ml three-necked flask, stir and heat up to dissolve completely, add 1g of activated carbon, continue to heat up to reflux, and stir for 1h to decolorize . Filtrate while it is hot, remove the act...

Embodiment 4

[0039] Add 20g of indomethacin crude product and 40g of acetone / water mixed solvent (the volume ratio of acetone to water is 1:1) into a 500ml three-neck flask, stir and heat up to dissolve completely, add 0.02g of activated carbon, continue to heat up to reflux, stir to decolorize 1h; filter while hot, remove activated carbon, obtain filtrate, filtrate is slowly cooled to 30°C, keep warm and crystallize for 10h, filter to obtain crystals, crystals are vacuum-dried at 50°C for 4h, and 16.8g of pure indomethacin is obtained, with a yield of 84.0% and a purity of 99.8 %.

Embodiment 5

[0041] Add 20g of indomethacin crude product and 300g of acetone / water mixed solvent (the volume ratio of acetone to water is 5:1) into a 500ml three-neck flask, stir and heat up to dissolve completely, add 0.6g of activated carbon, continue to heat up to reflux, stir to decolorize 1h; filter while hot, remove the activated carbon, obtain the filtrate, slowly cool the filtrate to -10°C, keep warm and crystallize for 6h, filter to obtain crystals, and dry the crystals in vacuum at 50°C for 4h to obtain 15.8g of pure indomethacin, with a yield of 79.0%. 100%.

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Abstract

The invention belongs to the field of drug synthesis, and relates to an indometacin purification method, which comprise the following steps of: mixing an indometacin crude product and a solvent, stirring, heating to achieve a dissolved state, carrying out active carbon decolorization treatment, carrying out cooling crystallization, filtering, and drying to obtain a high-purity indometacin pure product; wherein the solvent is one of an acetone / water mixed solvent, a tetrahydrofuran / water mixed solvent and an acetonitrile / water mixed solvent. According to the method, esterification of indometacin in the purification process is avoided, the purity of the prepared indometacin reaches 99.5% or above, and the maximum single impurity content is 0.1% or below.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a method for purifying indomethacin. Background technique [0002] Indomethacin (Indometacin, alias: indomethacin), chemical name: 2-methyl-l-(4-chlorobenzoyl)-5-methoxy-1H-indole-3-acetic acid, chemical formula: [0003] [0004] Indomethacin is a synthetic indole derivative, which is a prostaglandin biosynthesis inhibitor, has anti-inflammatory, anti-rheumatic, antipyretic, and relieving inflammatory pain effects, and is a commonly used clinical drug. [0005] At present, the purification method of indomethacin mostly adopts the recrystallization method, and the commonly used crystallization solvents are ethanol and methanol. Since indomethacin is an organic acid compound, the following esterification reaction will occur with the solvent during the purification process: [0006] [0007] The introduction of indomethacin methyl ester or indomethacin ethyl ester ...

Claims

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Application Information

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IPC IPC(8): C07D209/28
CPCC07D209/28
Inventor 苗向阳范许通徐圆亮李尚
Owner 河南优凯制药有限公司
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