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Easily available, six‐membered cyclic nitroso acetals 2 are smoothly oxidized with meta‐chloroperbenzoic acid to δ‐nitro alcohols 3 or γ‐nitro carbonyl compounds 4 with the retention of their relative configurations of stereocenters (diastereomeric ratio > 10:1). The reaction sequence – the generation of diastereomerically pure six‐membered cyclic nitronates 1 from simple aliphatic nitro compounds...
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