达沙替尼衍生物的合成及其产率分析

Synthesis and yield analysis of dasatinib derivatives

[目的]制备达沙替尼丁二酸单酯衍生物(DAS⁃SA)并建立分析产率的方法。[方法]采用核磁共振氢谱法确认达沙替尼丁二酸单酯衍生物的合成并采用高效液相色谱法(HPLC),以DAS为对照品间接测定产物中DAS⁃SA的百分含量(即纯度),最后对该反应的产率进行计算。[结果]达沙替尼丁二酸单酯衍生物被成功合成,且反应条件较为温和,通过高效液相色谱法定量分析得到反应产率为71.16%。[结论]建立的高效液相色谱法对DAS衍生物进行定量分析具有快速高效、专属性好、准确度高等优点,可为达沙替尼衍生物的含量测定提供方法依据。

[Objective]To prepare dasatinib succinic acid monoester derivative DAS⁃SA and establish a method for analyzing the yield.[Methods]the synthesis of dasatinib succinic acid monoester derivative was confirmed by 1H NMR and the percentage content purity of DAS⁃SA in the product was indirectly determined by high performance liquid chromatography HPLC with DAS as the control substance.Finally the yield of the reaction was calculated.[Results]Dasatinib succinate monoester derivatives were synthesized successfully and the reaction conditions were mild.The reaction yield was 71.16%by high performance liquid chromatography HPLC.[Conclusion]The highperformance liquid chromatography established in this experiment has the advantages of high speed high efficiency good specificity and high accuracy for the quantitative analysis of DAS derivatives which can provide a method basis for the determination of dashatinib derivatives.