Phosphorus-31 and two-dimensional phosphorus-31/proton correlated NMR spectra of duplex d(Ap[17O]Gp[18O]Cp[16O]T) and assignment of phosphorus-31 signals in d(ApGpCpT)2-actinomycin D complex

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Abstract
A solid-phase phosphoramide method was used for the synthesis of unlabeled and phosphoryl-labeled d(Ap-[17O]Gp[18O]Cp[16O]T [deoxy/(oxygen-17-labeled-adenylyl(3''-5'')oxygen-18-labeled-guanylyl(3'',5'')cytidylyl(3''-5'')thymidine]. The ability to label the phosphoryl oxygens of d(ApGpCpT) [duplex deoxy/adenylyl(3''-5'')guanylyl)3''-5'')thymidine] and thus assign the 31P signals, combined with a 2-dimensional 31P/1H chemical shift correlated NMR spectral technique, provided a novel means for the steady assignment of the H5'' and H3'' protons coupled to the phosphates. Phosphoryl labeling has also allowed the assignment of 31P NMR signals in the actinomycin D-d(Ap-[17O]Gp[18O]Cp[16O]T)2 duplex complex and confrim that the drug intercalates between the GpC stacked base pairs.
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