Aniline → Phenazine

Participants

Reaction Conditions

Reaction Steps

195.4 gms of calcined and protonated ZSM-5 was added to a mixture of 156.3 gms of 25% aqueous TMA(OH) and 195 ml of deionized water. The solution was ion exchanged for three hours at 40° C. using a hot water bath. The slurry was filtered and the filtrate was set aside for future loadings and ion exchange. The filter cake was subjected to further drying in a vacuum desiccator that was equipped with a nitrogen purge. The drying in the vacuum desiccator was at 35° C. and maintained at that temperature for several hours (48 hours or less) for complete removal of the moisture. The dried material was treated with 216.3 gms of 25% aqueous TMA(OH) for a 20% target loading of TMA(OH). The resulting slurry was dried in a rotary evaporator set-up for several hours until it was moist dry. The rotary evaporator was run at 35° C. and 4 to 35 mm Hg. The dried material was transferred to a flat dish and placed in a vacuum desiccator with an inert gas purge. The vacuum desiccator is maintained at 40° C. and drying was allowed for several hours (48 hours or less). The resulting dried material was not hard, and easy to grind and consisted of what appears to be one phase when ground. A coupling reaction test based on reacting aniline and nitrobenzene failed to produce phenazine.

Provenance & Evidence