Abstract The reaction of 5‐bromomethyl‐3‐(p‐bromomethylphenyl)isoxazole with o‐, m‐, and p‐bis(mercap‐tomethyl)benzenes gave the corresponding dithia‐ and/or tetrathiaisoxazolophanes, whose relative yields strongly depended upon the nature of the mercaptomethyl compound. The above isoxazole dibromide reacted with the bis(mercaptomethyl)isoxazole to afford a mixture of two isomeric dithiaisoxazolophanes.