Department of Chemistry, Yale University , New Haven, Connecticut 06520, United States.
Division of Chemical Sciences, Lawrence Berkeley National Laboratory, and Department of Chemistry, University of California , Berkeley, California 94720, United States.
J Am Chem Soc. 2016 Sep 28;138(38):12664-70. doi: 10.1021/jacs.6b08355. Epub 2016 Sep 19.
Multisubstituted tropanes and indolizidines have been prepared with high regio- and stereoselectivity by the [3+2] cycloaddition of unstabilized azomethine ylides generated from readily prepared trimethylsilyl-substituted 1,2-dihydropyridines via protonation or alkylation followed by desilylation. Starting from 1,2-dihydropyridines bearing a ring trimethylsilyl substituent at the 6-position, an intermolecular alkylation/desilylation provides endocyclic unstabilized ylides that successfully undergo cycloaddition with a range of symmetrical and unsymmetrical alkyne and alkene dipolarophiles to afford densely substituted tropanes incorporating quaternary carbons in good yields and with high regio- and stereoselectivity. Additionally, an intramolecular alkylation/desilylation/cycloaddition sequence provides convenient and rapid entry to bridged tricyclic tropane skeletons, allowing for five contiguous carbon stereocenters to be set in a single experimental operation and under mild conditions. Starting from 1,2-dihydropyridines with trimethylsilylmethyl groups on nitrogen, protonation followed by desilylation generates exocyclic unstabilized ylides that undergo cycloaddition with unsymmetrical alkynes to give indolizidines with good regio- and stereoselectivity. N-Trimethylsilylmethyl-1,2-dihydropyridines can also be alkylated and subsequently desilylated to give endocyclic unstabilized ylides that undergo intermolecular cycloadditions with carbonyl compounds to give bicyclic oxazolidine products in good overall yields. Moreover, an intramolecular alkylation/desilylation/cycloaddition sequence with the N-trimethylsilylmethyl-1,2-dihydropyridines affords tricyclic indolizidines that incorporate quaternary carbons and up to five stereocenters with good to excellent regio- and diastereoselectivity.
通过质子化或烷基化后脱硅,从容易制备的三甲基硅取代的 1,2-二氢吡啶生成未稳定的亚甲胺叶立德,高区域和立体选择性地制备了多取代的托烷和吲哚里嗪。从具有环三甲硅基取代基的 6-位的 1,2-二氢吡啶开始,通过烷基化/脱硅,提供内环未稳定的亚甲胺叶立德,该叶立德可以成功地与一系列对称和不对称的炔烃和烯烃偶极体进行环加成,以高产率和高区域选择性和立体选择性得到含有季碳原子的稠取代的托烷。此外,通过分子内烷基化/脱硅/环加成序列,提供了方便快速的方法来合成桥连的三环托烷骨架,允许在单个实验操作和温和条件下设置五个连续的碳立体中心。从具有氮上的三甲基硅基甲基的 1,2-二氢吡啶开始,质子化后脱硅生成外消旋的未稳定的亚甲胺叶立德,与不对称的炔烃进行环加成,以良好的区域和立体选择性得到吲哚里嗪。N-三甲基硅基甲基-1,2-二氢吡啶也可以被烷基化,然后脱硅,生成内环未稳定的亚甲胺叶立德,该叶立德与羰基化合物进行分子间环加成,以良好的总收率得到双环恶唑烷产物。此外,N-三甲基硅基甲基-1,2-二氢吡啶的分子内烷基化/脱硅/环加成序列得到含有季碳原子和多达五个立体中心的三环吲哚里嗪,具有良好到优异的区域和非对映选择性。