C-Aryl-N-phenylnitrones have been prepared in very high yields from N-phenylhydroxylamine and aryl aldehydes using the microwave irradiation technique within a few minutes. The synthesis of a new series of nitrones, viz. the series of C-aryl-N-(4′-chlorophenyl)nitrones were also achieved by this technique. Systematic and detailed spectroscopic investigations of all these nitrones were undertaken and some generalisations made regarding their spectroscopical properties.