利用Mitsunobu反应合成甲基三氯生-甲基-D_(3)

Synthesis of methyl triclosan-methyl-D_(3) by Mitsunobu reaction

研究了一种合成稳定同位素标记的甲基三氯生-甲基-D_(3)的新方法,即以三氯生和甲醇-D_(4)为起始原料,利用Mitsunobu反应合成得到甲基三氯生-甲基-D_(3),收率95.5%。产品结构、纯度和氘同位素丰度经核磁共振波谱(NMR)、气相色谱(GC)和质谱(MS)等仪器表征确定,甲基三氯生-甲基-D_(3)的色谱纯度和氘同位素丰度均高于99.0%。该化合物可以作为稳定同位素内标试剂,用于甲基三氯生的含量检测。

A new synthetic method of the stable isotope labeled methyl triclosan-methyl-D_(3) was investigated.The stable isotope labeled methyl triclosan-methyl-D_(3) in yield of 95.5%was synthesized by Mitsunobu reaction from triclosan and methanol-D_(4).The structure,chemical purity and isotopic enrichment of the product were identified by NMR,GC and MS to be the target compound.The chemical purity of GC and isotopic enrichment were higher than that of 99.0%in methyl triclosan-D_(3).The result showed that the methyl triclosan-methyl-D_(3) could be used as internal standard in the determination of methyl triclosan.