1, 3, 3-Trinitroazetidine (1) was synthesized and its structure elucidated by X-ray crystallography. Reaction of l-tert-butyl-& ((methylsulfony1) oxy) azetidine (3a) with sodium nitrite gave 1-tert-butyl-3-nitroazetidine (4a), which was converted to l-tert-butyl-3, 3- dinitroazetidine (5a) by oxidative nitration. Nitrolysis of 5a with acetyl nitrate gave 1. l- Benzhydryl-3, 3-dinitroazetidine (5b) did not undergo a similar nitrolysis. Single-crystal X- ...