A transition metal free oxidative C-H bond functionalization/esterification of α-alkoxy alkanes with acids is described in this report. This method is effectively mediated by NCS instead of traditional oxidants, like TBHP or its derivatives, and directly generates the esterification products in moderate to high yield under mild conditions. This tranformation constitutes a practical and general approach toward various α-acyloxy ethers with broad substrate generality; alkyl-, aryl-, alkenyl- and alkynyl-carboxylic acids are all well tolerated.
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