Very high inversion barriers for a pyramidal nitrogen atom have been found for the sterically hindered 1,2,4‐oxadiazolidines 1 (R1, R2=CH3) and 2 (R1=COOCH3, R2=CH2CH3, only one enantiomer is shown). The synthesis and NMR studies of the diastereomerization of 2 are described, as well as the determination of the enantiomerization barrier of 1 by stopped‐flow multidimensional gas chromatography (sfMDGC).
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