乙丙昔罗的合成工艺研究

摘要

目的 优选变构血红蛋白调节剂乙丙昔罗合成的反应条件.方法 采用正交设计法的4因素3水平的L9(34)试验方案进行试验和数据分析,选择最佳水平的工艺条件.结果与结论 优选出的合成条件为反应温度50℃,溶剂选用四氢呋喃,中间体(Ⅱ)与氢氧化钠的最佳摩尔比控制在1:5.5,所得目标化合物经IR、1H-NMR、LCMS谱确证,且总收率为78.3％.该方法反应条件温和,反应时间短,操作简便,收率高,适合工业化生产.%Objective To screen the factors of the synthesis for allosteric modifiers of hemoglobin,efaproxiral.Methods According to the orthogonal design method,four factors and three levels were adopted to synthesis of efaproxiral,and screen out the optimum condition after the experiment and analysis.Results and Conclusion The optimum condition was as follows:temperature(50℃),solvent(THF),and the molar ratio of intermediate and sodium hydroxide (1:5.5),the structure of the compound was confirmed by IR,1H-NMR and LC-MS,the total yield was 78.3％.This method has the advantages of good yields,short reaction time,easy preparation and mild reaction conditions.It is suitable for industrial production.