Outlines and discusses procedures for the preparation of lucigenin, a powerfully chemiluminescent compound. Major techniques (requiring three 4-hour sessions) involving nucleophilic and electrophilic aromatic substitution, nucleophilic aliphatic substitution, reductive coupling, and oxidation reactions include steam distillation, decolorization with charcoal, Soxhlet extraction, dipolar solvent use enhancing ionic reactions, and vacuum distillation. (Author/JN)