Divergent synthesis of Haplomitrium diterpenoids via a late-stage biomimetic skeletal reorganization approach

通过后期仿生骨架重组方法实现哈普洛米特里二萜类化合物的发散合成

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Abstract

Labdane-type terpenoids, the large super-family of diterpenoids, exhibit diverse biological significance. Labdane-derived hapmnioide-type diterpenoids, which have been identified as chemical markers for Haplomitrium liverwort, show potent anti-inflammatory and allelopathic activities. Biosynthetically, their structural complexity and diverse carbon skeletons arise from cascade ring mutations. We describe total synthesis of seven typical Haplomitrium diterpenoids through late-stage biomimetic skeletal reorganization, featuring 1,2-acyl migration, tandem C5-isomerization/aldol/retro-Claisen reactions, and light-initiated [2 + 2] cyclization. A diastereoselective intramolecular Diels-Alder reaction is employed to rapidly assemble the common labdane core skeleton. The 1,2-migration of the labdane intermediate is developed to synthesize hapmnioide A and haploide O. Furthermore, the tandem C5-isomerization/aldol/retro-Claisen reactions and light-initiated [2 + 2] cyclization of the common labdane intermediate enables the reconstruction of haploide C and haplomitrins A/C, respectively. The synthetic work provides mechanistic insights into the biosynthesis of hapmnioide-type diterpenoids. Further investigations of the 1,2-acyl migration of other terpenoids demonstrate the general and potential applicability of such late-stage rearrangements for the synthesis of homologous molecules.

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