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An efficient, scalable and operationally simple one-pot, 2-step strategy for the nucleophilic formylation of\udtrifluoromethyl ketones is presented. The key step is an unprecedented diaza-carbonyl-ene reaction of\udformaldehyde tert-butyl hydrazone and trifluoromethyl ketones under solvent-free conditions. This reaction\udproved to be very fast, clean and high-yielding, affording densely functionalised α-hydroxy\udα-trifluoromethyl diazenes. The ensuing diazene-to-aldehyde transformation, avoiding protection/deprotection\udreactions and chromatographic purifications, and subsequent derivatizations in a one-pot\udfashion provide a direct entry to a variety of useful trifluoromethylated building blocks.We acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI).This work was supported by the Ministerio de Economía y\udCompetitividad of Spain (CTQ2013-48164-C2-1-P, CTQ2013-48164-C2-2-P, and predoctoral fellowship to E. M.), European FEDER funds and the Junta de Andalucía (Grant 2012/FQM 1078). D. M. acknowledges Universidad de Sevilla for a postdoctoral\udcontract.Peer reviewe

Solvent-free synthesis of quaternary α-hydroxy α-trifluoromethyl diazenes: the key step of a nucleophilic formylation strategy