Summary The cleavage and functionalization of carbon-carbon (C–C) bonds has emerged as a powerful tool for preparing value-added chemicals. In this protocol, we describe the preparation of amorphous manganese oxide and its application as a heterogeneous catalyst in the direct synthesis of amides via successive cleavage and amidation of C–C bonds in alcohols. Furthermore, we describe how a slight modification of reaction conditions allows for the cleavage and cyanation of alcohols to access sterically hindered nitriles. For complete details on the use and execution of this protocol, please refer to He et al. (2022) .
Ting Zhang,Weitao Wang,Meng He,Huan Wang,Zhen-Hong He,Yang Yang,Kuan Wang,Zhao-Tie Liu
Imines as valuable chemical intermediates can be synthesized by aerobic photocatalytic oxidation of amines, which is recognized as a promising and green route for imines synthesis. It is attractive to develop solvent-free photocatalytic oxidation of amines with high efficiency, especially with high activity and selectivity, but it is challenging. In the present work, flower-like BiOX/TiO 2 (X = Cl, Br, I) heterojunction was designed for solvent-free photocatalytic oxidation of benzylamine to N-benzylidenebenzylamine. Type II heterojunction of BiOCl/TiO 2 with 67.3 wt% of BiOCl achieved the high formation rate of 6316 µmol∙g −1 ∙h −1 and selectivity of 99 % on BiOCl/TiO 2 . To the best of our knowledge, the activity and selectivity are the highest for solvent-free photocatalytic system. The reason for the varied photocatalytic performances were investigated. The solvent-free photocatalytic mechanism was revealed and proposed. Moreover, the BiOCl/TiO 2 photocatalyst can be used for photocatalytic oxidation of varied benzylamines to imines.