Evolution of the Short Enantioselective Total Synthesis of the Unique
Marine Myxobacteria Polyketide Salimabromide
Abstract
Salimabromide, a unique and scarce marine tetracyclic polyketide, was
synthesized in both racemic and optically active forms. A novel
carboxylic acid-directed method for tandem oxidative difunctionalization
of olefins was developed, whereby the formation of bridged butyrolactone
and enone moieties occurs concurrently. Density functional theory (DFT)
calculations indicate that this reaction follows a [3+2] process
rather than the [2+2] process. In the meantime, the distinctive
benzo-fused [4.3.1] carbon skeleton and highly hin-dered vicinal
quaternary stereocentres were simultaneously constructed through a
challenging intramolecular Giese-Baran radical cyclization. Furthermore,
deuterium kinetic isotopic effects were utilized to enhance the efficacy
of this pivotal step. This represents a new illustration of the
application of kinetic isotope effects in natural product synthesis.
Then, short asymmetric syntheses of (+)-salimabromide (13 or 15 steps)
was accomplished by combing this method with rhodium-catalyzed
enantioselective hydrogena-tion of a cycloheptenone derivative (97% ee)
or conjugate addition of an aryl boronic acid with 2-cyclohepten-1-one
(> 99% ee).