Caleb E. Griesbach,Jean‐Nicolas Desrosiers,Liam S. Sharninghausen,Teresa W. Makowski,Steven M. Guinness,Ethan Wood,Chase A. Salazar,Caleb J. Kong,Jenson Verghese
A Ni-catalyzed cross-coupling is utilized as a reversed strategy for the homogeneous deprotection of benzyl ethers. The reaction is accelerated in batch using microwave heating or in flow using superheating in a plug flow reactor to achieve the desired (hetero)aromatic alcohols bearing heterocycles, alkenes, and ethers within 1 h. This work highlights an alternative debenzylation strategy in flow for cases where hydrogenation using heterogeneous catalysts is not a viable option.