Abstract:A novel DTBP‐promoted Passerini‐type reaction of isocyanides with two molecular aldehydes has been developed. This reaction is applicable for a wide range of isocyanides and aldehydes and provides an efficient method for the synthesis of α‐acyloxycarboxamides with two identical functional groups in good to high yields in a single step. The experimental results clearly confirmed the role of water and provided a better mechanistic understanding of this reaction.
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