双烯醇酮醋酸酯主要杂质的合成研究

Synthesis of Major Impurity of 16-DPA

将双烯醇酮醋酸酯溶于苯中,加入过氧化叔丁醇、重铬酸吡啶盐、硅藻土,于室温反应2~3 h,得到杂质粗品;粗品经层析柱分离,乙醇、二氯甲烷精制,得到主要杂质化合物Ⅰ;其结构经1H NMR和ESI-MS确证。

Dissolving 16-DPA in benzene and adding tert-butyl hydroperoxide, PDC, diatomite, keeping the reaction at room temperature for 2~3 h, we get crud impurity; we get compound Ⅰ when the crud impurity is separated by glass chromatography column and purified by ethanol and dichloromethane. The structure was confirmed by 1H NMR and ESI-MS.