Unsymmetrical diphosphenes carrying bulky aryl and phenoxy groups were prepared by the reaction of lithium 2,4,6‐tri‐t‐butylphenylphosphide with the corresponding phenyl phosphorodichloridites, followed by the dehydrochlorination reaction with 1,8‐diazabicyclo[5.4.0]undec‐7‐ene. The diphosphenes were isolated as stable compounds. The reactions of these diphosphenes with elemental sulfur or selenium afforded the corresponding thiadiphosphiranes or selenadiphosphiranes, respectively. The diphosphenes also reacted with dichlorocarbene to give dichlorodiphosphiranes.
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