Herein, we report a straightforward protocol for the preparation of N,N-dimethylated amines from readily available nitro starting materials using formic acid as a renewable C source and silanes as reducing agents. This tandem process is efficiently accomplished in the presence of a cubane-type Mo PtS catalyst. For the preparation of the novel [Mo Pt(PPh )S Cl (dmen) ] (3 ) (dmen: N,N'-dimethylethylenediamine) compound we have followed a [3+1] building block strategy starting from the trinuclear [Mo S Cl (dmen) ] (1 ) and Pt(PPh ) (2) complexes. The heterobimetallic 3 cation preserves the main structural features of its 1 cluster precursor. Interestingly, this catalytic protocol operates at room temperature with high chemoselectivity when the 3 catalyst co-exists with its trinuclear 1 precursor. N-heterocyclic arenes, double bonds, ketones, cyanides and ester functional groups are well retained after N-methylation of the corresponding functionalized nitroarenes. In addition, benzylic-type as well as aliphatic nitro compounds can also be methylated following this protocol.
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