Solid-phase synthesis of hydroxypiperazine derivatives using phenethylamine linker by oxidation–Cope elimination
作者:Jin-soo Seo、Hye-won Kim、Cheol Min Yoon、Deok Chan Ha、Young-Dae Gong
DOI:10.1016/j.tet.2005.07.061
日期:2005.9
90 °C for 2 h. The utility of the methodology for solid-phase synthesis of general hydroxylamines was also investigated using the same linker. The progress of reactions could be monitored on polymer bound intermediates by ATR-FTIR spectroscopy on single bead. The desired products were obtained in good six-step overall yields upon cleavage from the resins and were characterized by LC/MS, 1H NMR, and 13C
据报道,一种基于m- CPBA的聚合物结合的苯乙胺连接基的氧化-Cope消除反应可以并行固相合成羟基哌嗪衍生物。苯乙胺N的关键中间体-氧化物树脂可在固相上分离,用于随后的β-消除,由此可以在90°C下保持2 h的高纯度和高收率获得所需的羟基哌嗪产品。还使用相同的接头研究了固相合成一般羟胺的方法学的实用性。可以通过在单个珠子上的ATR-FTIR光谱监测在聚合物结合的中间体上反应的进程。从树脂上裂解后,以良好的六步总产率获得了所需的产物,并通过LC / MS,1 H NMR和13 C NMR光谱对其进行了表征。