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One‐pot intramolecular cyclization of novel sp3‐enriched cyanoalkylsulfonyl fluorides into spirocyclic β‐ or γ‐sultams is disclosed. The method relies on nitrile group reduction followed by sulfonylation of amino group thus formed upon mild conditions (NaBH4, NiCl2·6H2O in MeOH). Cyclization proceeds smoothly with considerable efficiency (48–84 %, 10 examples) on up to 30 g scale. The cyanoalkylsulfonyl...
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