CAJ | 학술논문

综述了国内外去甲基阿奇霉素的合成路线,研究了去甲基阿奇霉素的制备工艺,探讨了重结晶溶剂种类、氧化剂、还原剂种类以及pH值等对反应效果的影响.结果表明,以甲醇为反应体系,在回流下用双氧水氧化,亚硫酸氢钠还原,反应结束后用氨水调节pH值至10.0,粗品用丙酮和水混合体系精制,产品纯度通过HPLC检测达到99.4%.
종술료국내외거갑기아기매소적합성로선,연구료거갑기아기매소적제비공예,탐토료중결정용제충류、양화제、환원제충류이급pH치등대반응효과적영향.결과표명,이갑순위반응체계,재회류하용쌍양수양화,아류산경납환원,반응결속후용안수조절pH치지10.0,조품용병동화수혼합체계정제,산품순도통과HPLC검측체도99.4%.
The synthesis process line of 3'-N-Demethyl azithromycin synthesis research at home and abroad is reviewed,and the method for 3'-N-Demethyl azithromycin is studied. The effect of solvent,oxi-dant, reductant,pH,etc. is discussed. The results that with methanol as solvent,using H2O2 as oxidant at reflux,and using NaHSO3 as reductant,after the immunoreaction,pH is adjusted to 10.0 with ammonia. Re-crystallization is prepared with acetone and water. The purity of product is as high as 99.9% according to the determination by HPLC.