保泰松钙的合成及条件优化  

Synthesis of phenylbutazone calcium and its condition optimization

作　　者：严宾 吴玉祥 

机构地区：[1]精华制药集团南通有限公司,江苏南通226407

出　　处：《现代医药卫生》2015年第19期2906-2907,2910,共3页Journal of Modern Medicine & Health

摘　　要：目的研究保泰松钙的合成方法 ,确定合成工艺中关键参数。方法以保泰松为原料,经碱液溶解及成钙盐两步合成保泰松钙,并分别从氢氧化钠加入量、活性炭脱色温度、乙酸钙加入量及滴加温度和甲基叔丁基醚洗涤温度这5个条件对保泰松钙的合成产率及纯度进行研究。结果优化条件:氢氧化钠加入量为30.0 g、脱色温度为50.0℃、乙酸钙加入量为134.4 g、乙酸钙滴加温度为50.0℃及甲基叔丁基醚洗涤温度为40.0℃,经过优化使得保泰松钙的合成回收率提升至98.6%,纯度达99.7%。结论该优化方法操作简单,反应条件温和且合成得到的保泰松钙结构经质谱和核磁共振证实。Objective To study the synthetic method of phenylbutazone calcium and to determine the key parameters of synthetic technology. Methods With phenylbutazone as the raw material,phenylbutazone calcium was synthesized by dissolution with alkaline solution and calcium salt forming. The yield rate and purity of phenylbutazone calcium synthesis were researched from the 5 conditions of the adding amount of sodium hydroxide,active carbon decolorization temperature,adding amount of calcium acetate and dropwise adding temperature and washing temperature of methyl tertiary butyl ether. Results The optimized conditions were the sodium hydroxide mass of 30.0 g,the decolorization temperature of 50.0 ℃,the calcium acetate amount of 134.4 g,and the dropwise add temperature of calcium acetate was 50.0 ℃ and the wash temperature of 40.0 ℃. The recovery rate of phenylbutazone calcium synthesis by optimization was increased to 98.6% and the purity was reached to 99.7%. Conclusion This method is easy to operate and its reaction condition is gentle,moreover the structure of synthesized phenylbutazone calcium is verified by the mass spectrum and nuclear magnetic resonance（NMR）.

关 键 词：药用制剂/化学合成 工艺学 制药 消炎药 非甾类 保泰松 条件优化 

分 类 号：R914.5[医药卫生—药物化学]