CAJ | 학술논문

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。
목적：연구보태송개적합성방법，학정합성공예중관건삼수。방법이보태송위원료，경감액용해급성개염량보합성보태송개，병분별종경양화납가입량、활성탄탈색온도、을산개가입량급적가온도화갑기숙정기미세조온도저5개조건대보태송개적합성산솔급순도진행연구。결과우화조건：경양화납가입량위30.0 g、탈색온도위50.0℃、을산개가입량위134.4 g、을산개적가온도위50.0℃급갑기숙정기미세조온도위40.0℃，경과우화사득보태송개적합성회수솔제승지98.6%，순도체99.7%。결론해우화방법조작간단，반응조건온화차합성득도적보태송개결구경질보화핵자공진증실。
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 ac-etate 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).