Synthesis of the 4‐Pyridine Analog of Kostanecki's Triketone. Determination of Constitution and Stereochemistry by 2D‐NMR Spectroscopy and X‐ray Structural Analysis

4‐Acetylpyridine reacts stereoselectively with benzaldehyde under basic conditions to afford rac‐1. The constitution of 1 was determined by the long‐range connectivities revealed by the H, C‐COLOC spectrum. The relative stereochemistry of the chiral centers C‐2 to C‐6 was obtained from ³J_HH couplings. The stereochemistry at the non‐proton bearing C‐1 was established by through‐space connectivities from ROESY and semiquantitative analysis of ³J_CH from an inverse 2D‐NMR spectrum (HMBC). The NMR findings were confirmed by single crystal X‐ray diffraction.