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Selective transfer hydrogenation (TH) of unsaturated molecules using methanol is challenging as the in situ generated formaldehyde is prone to react with the active methylene (C-methylation) or amine (N-methylation) core...

In this work, a single‐atom cobalt‐catalyzed transfer hydrogenation (TH) of azides is reported under mild conditions (at 30 °C in 30 min) using NH2NH2 ⋅ H2O as the hydrogen source. Employing this protocol, a wide range of azides were transformed to their corresponding amines. This methodology was extended towards the synthesis of several important N‐substituted pyrroles from azides in one‐pot manner. The control experiments suggested, the transfer hydrogenation favoured by electron withdrawing substituents and one‐pot pyrrole synthesis favoured by electron‐donating substituents. The recyclability test revealed the catalysts could be recycled up to 7th times without significant loss in the catalytic activity.