Aniline → Phenazine

Participants

Reaction Conditions

Reaction Steps

This example is similar to TMA(OH) loading Example No. 7 except that the slurry contained 262.4 gms of calcined and protonated ZSM-5, 211.4 gms. Of 25% aqueous TMA(OH) and 262 ml of deionized water. The ion exchange was conducted at 40° C. for three hours. The filter cake after ion exchange was dried using a vacuum desiccator without a nitrogen purge overnight at room temperature. The drier cake was further dried in a vacuum desiccator at 35° C. for 2.5 hours using a nitrogen purge. For a 20% target loading of TMA(OH) onto the ZSM-5, 413.8 gms of 25% aqueous TMA(OH) was added into a vessel that was connected to an assembly that was similar to a rotary evaporator. The hot water bath was maintained at about 35° C. and the drying/evaporating process was conducted for about 2.5 hours at vacuum pressures between 8 and 38 mm Hg. The dried material was removed from the vessel and transferred to a flat dish for further drying in a vacuum desiccator. The drying in the vacuum desiccator was kept at 40° C. for about 3 hours. 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