Abstract
A sustainable protocol has been devised for the oxidation of activated secondary alcohols to their corresponding carbonyl compounds, as well as their utilization as selective mono‐alkylating reagents for both amide and arylsulfonamide derivatives. These reactions proceed smoothly and in good yields (up to 98%) when conducted in Fe‐based deep eutectic solvents (DESs), which serve dual roles as solvents and catalysts. Operating under mild (40 °C) and aerobic conditions, these transformations are completed within a 4 h time frame. A pharmacologically relevant amide derivative, specifically a PMRT1 inhibitor, has also been successfully synthesized on a 3 g‐scale utilizing a reusable FeCl3·6H2O/glycerol Lewis acidic DES.
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