Aniline → Phenazine

Participants

Reaction Steps

116.0 gm of calcined and protonated ZSM-5 was added to a solution of 92.8 gms of 25% aqueous TMA(OH) and 116 ml of deionized water. The resulting slurry was ion exchanged for about 4 hours at 48° C. The slurry was filtered in a Buchner funnel. The filter cake was dried at 40° C. in a vacuum desiccator for fourteen hours and the filtrate set aside for use in subsequent loading. To the dried filter cake was added 122.7 gms of 25% aqueous TMA(OH). The resulting slurry was vigorously mixed at 40 ° C. for 30 minutes and dried in a vacuum desiccator for 72 hours with no inert gas purge. An additional 48 hours of drying at room temperature yielded a very hard solid material that was very difficult to grind. The ground solid consisted of what appeared to be two solid phases. A coupling reaction of aniline and nitrobenzene using the ground material from this preparation produced appreciable levels of phenazine.

Provenance & Evidence