Several studies for the synthesis of polycyclic derivatives have been reported; however, there is little information on the preparation of steroid‐polycyclic derivatives. In this way, the aim of this study was to synthesize a bismethylsulfanyl‐steroid‐azetyl butanol derivative (compound 10) from 2‐nitroestrone. The chemical structure was evaluated through both 1H NMR and 13C NMR or spectroscopic analysis. The results showed a good yielding from 10. It is noteworthy that the reagents used in this investigation are not expensive and do not require special conditions for handling.