The synthesis, by green methodology using microwaves, of the novel Schiff base LH derived from o -vanillin and acetazolamide and of the corresponding organotin derivatives R 2 SnL 2 (1, R = n -Bu; 2, R = n -Oct) and n -Bu 3 SnL (3) is reported. The compounds are characterized by elemental analyses; 1 H, 13 C, and 119 Sn NMR; IR; and UV-vis spectroscopy.