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.