Parecoxib sodium genetic toxicity impurity and preparation method of same

The invention relates to a parecoxib sodium genetic toxicity impurity and a preparation method of same. The preparation method includes: at -5 to 0 DEG C, mixing 5-methyl-3,4-diphenyl isoazole and dichloromethane and adding chlorosulfonic acid at the rate of lower than 3 ml/min, and monitoring the r...

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Hauptverfasser: DU DIZHENG, ZHANG YAN, QI CHUANGYU, LUO GUOJUN, YAN HONGYING, ZHONG HUI
Format: Patent
Sprache:chi ; eng
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Zusammenfassung:The invention relates to a parecoxib sodium genetic toxicity impurity and a preparation method of same. The preparation method includes: at -5 to 0 DEG C, mixing 5-methyl-3,4-diphenyl isoazole and dichloromethane and adding chlorosulfonic acid at the rate of lower than 3 ml/min, and monitoring the reaction process through high performance liquid chromatography to obtain a reaction liquid; quenching and extracting the reaction liquid, adding a methanol solution of sodium methoxide, an ethanol solution of sodium ethoxide or an isopropanol solution of sodium isopropoxide to perform a reaction for2-4 h to obtain 4-(5-methyl-3-phenyl-4-isoxazolyl)methyl benzenesulfonate, 4-(5-methyl-3-phenyl-4-isoxazolyl)ethyl benzenesulfonate or 4-(5-methyl-3-phenyl-4-isoxazolyl)isopropyl benzenesulfonate. The three parecoxib sodium genetic toxicity impurities are more than 99.5%, even 99.73%, in purity. The method can reach more than 67%, even 71.0%, in yield. 本发明涉及一种帕瑞昔布钠遗传毒性杂质及其制备方法。制备方法包括:于温度-5℃~0℃下,混合5-甲基-3,4-二苯基异恶唑和二氯甲烷,再<3