As the first step towards the biosynthetic studies on grayanotoxins with the aid of 13C isotope, the 13C-NMR spectra of grayanotoxin-I and III were assigned. Unambiguous assignments were achieved except for the C-9 and C-I 3 resonances in G-I by selective proton decoupling technique as well as by comparison with chemical shift values of the related com-pounds.
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