Abstract

AbstractAn efficient, LiN(SiMe3)2‐mediated phosphorylation of terminal alkynes with chlorodiphenylphosphine oxide has been developed to synthesize alkynylphosphine oxides. This transition‐metal‐free protocol was featured with simple operation, mild reaction conditions, and broad substrate scope. The tolerance of halogen and ester substituents displayed the advantages of this new method over the traditional ones. In addition, the application potential was demonstrated by the gram‐scale reaction. When using diisopropyl chlorophosphate and chlorodiphenylphosphine, the corresponding alkynylphosphate and alkynylphosphine could also been produced.

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