Key Laboratory of Bioorganic Phosphorus Chemistry and Chemical Biology (Ministry of Education), Department of Chemistry, Tsinghua University, Beijing 100084, People's Republic of China.
J Org Chem. 2010 Mar 19;75(6):1911-6. doi: 10.1021/jo902615u.
A general method for the preparation of enantiopure 2-alkene- or 2-alkyne-containing chain substituted piperidines was established by using nonracemic Betti base as a chiral auxiliary. The key step is that the auxiliary residue was removed by a novel base-catalyzed N-debenzylation via a formation of o-quinone methide mechanism in stead of the traditional hydrogenolysis, by which the alkene or alkyne groups survived. By this method, ten 2-alkene- or 2-alkyne-containing chain substituted piperidines were prepared on the gram scale within a few hours. To demonstrate the efficiency of the method and the versatility of the product, total syntheses of natural alkaloids (+)-pelletierine, (-)-lasubine II, and (+)-cermizine C were achieved by using (S)-2-allyl-N-Boc-piperidine as a versatile building block.
建立了一种通用的方法,通过使用非手性的 Betti 碱作为手性辅助剂,制备对映纯的 2-烯烃或 2-炔烃取代的哌啶。关键步骤是通过新型碱催化的 N-去苄基化反应,通过形成 o-醌甲醚机制,而不是传统的氢化反应,来去除辅助残基,从而使烯烃或炔烃基团得以保留。通过这种方法,在几小时内以克级规模制备了十个 2-烯烃或 2-炔烃取代的哌啶。为了证明该方法的效率和产物的通用性,通过使用(S)-2-烯丙基-N-Boc-哌啶作为多功能构建块,实现了天然生物碱(+)-pelletierine、(-)-lasubine II 和(+)-cermizine C 的全合成。