The Challenging Complete and Detailed (1)H and (13)C NMR Assignment for ent-Kaurenoic Acid, a Remarkable Natural Product

对一种卓越的天然产物ent-Kaurenoic Acid进行具有挑战性的完整且详细的(1)H和(13)C NMR谱图归属

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Abstract

In this work, we report a comprehensive structural assignment of the (1)H and (13)C nuclear magnetic resonance (NMR) data for kaurenoic acid (KA, ent-kaur-16-en-19-oic acid), a natural diterpene with diverse biological activities. To support this analysis, the methyl ester derivative (ent-methyl-kaur-16-en-19-oate) was also investigated, allowing comparison of chemical shift variations arising from subtle structural differences. The complete assignment was achieved through the analysis of multidimensional NMR spectra and accurate determination of (1)H-(1)H coupling constants and signal multiplicities. Experiments including (1)H NMR, (13)C NMR {(1)H}, g-COSY, g-HSQC, g-HMBC, and J-resolved were employed, complemented by spectral simulations using FOMSC3 and SimEsp_NMR software. Measurements in different deuterated solvents further clarified overlapping regions and enhanced data reliability. This approach resulted in the most detailed and complete NMR data set to date for KA and its methyl ester. To our knowledge, no previous studies on KA have provided this level of spectroscopic detail or a step-by-step description of the data acquisition, underscoring the novelty and relevance of this work.

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