Fine purification method for ampiroxicam

Abstract

An ampiroxicam refining method comprises the following steps: dissolving crude ampiroxicam product in ketone or alcohol at a ratio of 10-35ml / g, and adding activated carbon which is 5-20% of the crude ampiroxicam product by mass; then adding silica gel which is 5-20% of the crude ampiroxicam product by mass for adsorption bleaching, filtering, and finally adding water to the crude ampiroxicam product at a ratio of 10-35ml / g, and performing crystallization, crystal cultivation and filtration to obtain white ampiroxicam crystal. The refined ampiroxicam produced by the method has the advantages of having good appearance, high quality, purity of 99.2% at least and content greater than 99.5%, and being suitable for clinical administration required for patients.

Description

Technical field: [0001] The invention relates to a method for refining ampiraxicam. Background technique: [0002] Ampiroxicam (Ampiroxicam, Flucam) is an Oxacam-like NSAID jointly developed by Pfizer and Toyama. It is a prodrug of piroxicam and is a cyclooxygenase inhibitor. It is a new generation of long-acting non-steroidal anti-inflammatory drugs. It is mainly used clinically for analgesia and pain relief after rheumatoid arthritis, osteoarthritis, low back pain, frozen shoulder, neck, shoulder and wrist syndrome, trauma, surgery and tooth extraction. Anti-inflammatory. 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. [0003] US4927921 reported the refining method of ampiraxicam. After the reaction solution containing the crude ampiraxicam was subjected to silica gel column ch...

AI Technical Summary

Problems solved by technology

These two methods have all used column chromatography, need to use a large amount of organic solvents to rinse, pollute seriously, be unfavorable for suitability for industrialized production, and recrystallization have used the limited solvent such as dioxane, diethyl ether, toluene, toxicity Large, high boiling point, easy to cause solvent residue, not conducive to the use of patients

[0004] CN1800180 has reported another kind of refining process, dissolving the crude product of ampiraxicam in haloalkane, washing, drying, evaporating to dryness and recrystallization, this process eliminates the toxic solvent toluene, without column chromatography, and the process is basically suitable for industrial production, but The process is relatively cumbersome, the consumption of solvent and power is large, and the yield is also low