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Ampiroxicam refining method

A technology of ampiraxicam and its refining method, which is applied in the direction of organic chemistry, can solve the problems of difficult removal of impurities, residual solvent, long time spent in column chromatography, etc., and achieve the effect of good appearance and high purity

Inactive Publication Date: 2008-05-21
NANJING YOKO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses toluene, which has strong carcinogenicity, as a recrystallization solvent, which is prone to solvent residues, difficult to remove impurities, and affects product quality. It is difficult to meet human clinical drug requirements.
In addition, column chromatography takes a long time, and the eluent used is a mixed solvent, which is not easy to recycle and apply mechanically, the cost is high, and it is difficult to realize industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 1000ml four-necked bottle equipped with a reflux condenser and a stirring rod, under nitrogen protection, add the crude product of ampiraxicam (12.3g), add 246ml of dichloromethane and stir to dissolve, wash with 125ml of water and 125ml of saturated saline respectively , dried over anhydrous sodium sulfate, evaporated dichloromethane, added 123ml of ethyl formate and 1.0g of activated carbon to the residue, refluxed for 30 minutes, filtered hot, cooled and crystallized, filtered, and dried under vacuum below 100°C to give ampiraxicam white 9.4 g of crystals, mp 157-159°C, yield 76.4%.

Embodiment 2

[0014] In a 1000ml four-neck bottle equipped with a reflux condenser and a stirring rod, under nitrogen protection, add the crude product of ampiraxicam (12.3g), add 123ml of bromobutane and stir to dissolve, wash with 230ml of water and 230ml of saturated saline respectively , dried over anhydrous sodium sulfate, distilled off bromobutane, added 62ml butanone and 1.0g activated carbon to the residue, refluxed for 25 minutes, filtered, cooled and crystallized, filtered, vacuum dried below 100°C, and white crystals of ampiraxicam 9.0 g, mp156~159°C, yield 73.2%.

Embodiment 3

[0016] In a 1000ml four-necked bottle equipped with a reflux condenser and a stirring rod, under nitrogen protection, add the crude product of ampiraxicam (12.3g), add 369ml of bromodecane and stir to dissolve, wash with 320ml of water and 320ml of saturated brine respectively , dried over anhydrous sodium sulfate, distilled off bromodecane, added 185ml of isopropanol and 1.0g of activated carbon to the residue, refluxed for 20 minutes, filtered, cooled and crystallized, filtered, and vacuum-dried below 100°C to obtain white crystals of ampiraxicam 8.9g, mp 155-158°C, yield 69.7%.

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PUM

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Abstract

The invention relates to a method for refining an bixi kang. It provides a new refining method which dissolves a bixi kang into the haloalkane, cleans, dries, condensations it and re-crystallizes it to obtain the bixi kang white crystallization.

Description

technical field [0001] The invention relates to a method for refining ampiraxicam. Background technique [0002] Ampiroxicam is 4-[1-(Ethoxycarbonyloxy)ethoxy]-2-methyl-N-2-pyridyl-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide (CAS Registry Number: 99464-64-9), is a new generation of long-acting non-steroidal anti-inflammatory drugs, mainly used clinically for rheumatoid arthritis, osteoarthritis, low back pain, frozen shoulder, neck, shoulder and wrist syndrome, trauma, Analgesic and anti-inflammatory after surgery and tooth extraction. As a new generation of non-steroidal anti-inflammatory analgesics taken once a day, ampiraxicam has strong effects, long duration, high safety, and good gastrointestinal tolerance, and has attracted much attention in the pharmaceutical market. EP 147177 reports the purification method of ampiraxicam: the reaction solution containing the crude ampiraxicam is subjected to column chromatography, and then recrystallized with toluene. This me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/12
Inventor 孙晋瑞王玉喜
Owner NANJING YOKO PHARMA
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