| Summary: | Abstract A facile method to prepare one‐dimensional (1D) organometallic nanomaterials from various ethynyl‐substituted molecules is reported. The reactions of 3‐chloro‐1‐ethynylbenzene, p‐tBu‐phenylacetylene and 4‐ethynylbiphenyl with Cu+ ions in acetonitrile yield nanorod‐shaped copper acetylides (Cu−C≡C−R) crystals. In the case of linear alkynes, namely, propyne, 1‐pentyne and 1‐hexyne, it was found that using an aqueous ammonia/ethanol mixed solvent instead of acetonitrile is a better approach to obtain 1D nanostructures. This procedure also enables us to prepare functional 1D nanomaterials. We demonstrate the preparation of a paramagnetic nanorod from the organic radical p‐ethynylphenyl nitronyl nitroxide, and fluorescent nanorods from 9‐ethynylphenanthrene and 2‐ethynyl‐9,9′‐spirobifluorene.
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