Some 5-nitrophenylfurane-2-aldehydes, 5-nitrophenylthiophen-2-aldehydes and two phenylhidrazones were synthesized. The 1 H-nMR, 13C-NMR and 2D-NMR spectra were assignted in DMSO by 500 MHz–NMR spectrometer. The spectra showed the influence of NO2–group to the chemical shift of 1 H- and 13C of the molecules.