The syntheses of 1,6-hexanedisulfonyl azide, 1,10-decanedisulfonyl azide, 1,3-benzenedisulfonyl azide, 1,5-naphthalenedisulfonyl azide, 2, 6-naphthalenedisulfonyl azide, and 4,4'-biphenyldisulfonyl azide are described in this article. The compounds are characterized according to their melting temperature, infrared spectra, mass spectra, and carbon-13 and proton nuclear magnetic resonance spectra, with the intention of assessing their potential as crosslinking agents for textile fibers.