Practical synthetic approaches to the new class of acetylenic derivatives of 3-imidazolyl-3- oxide-1-oxyls, including biradicals, were developed through cross-coupling reactions of 3- imidazolyl halides with either terminal alkynes or their copper salts. The presence of nitroxyl functional group as an internal oxidant leads to a competition between the formation of cross- coupling products and the products of oxidative homocoupling. The balance in this ...