Oxygen → HCID 19044959, compound

Participants

Reaction Conditions

Reaction Steps

A phenolic solution (feedstream A) was prepared consisting of 1.7849 g Pd(acac)2 (5.86 mmol), 20.14 g PbO (90.2 mmol; 15.4 equivalents of lead per equivalent of palladium) and 11.4 liters of phenol. A second phenolic solution (feedstream B) was prepared consisting of 1261 g hexaethylguanidinium bromide (4112 mmol) in 3.2 liters of phenol. Each feedstream was maintained at 65° C. and pumped at a rate of 1.5 liters/hour into a stirred, 1-gallon continuous reactor system, maintained at 65° C. and 40 psig. Once the reactor was filled, gas flow of a mixture consisting of 6% oxygen in carbon monoxide was initiated at a rate of 1200 SLPH to achieve a pressure of 1200 psig, after which the reactor temperature was increased to 100° C. These conditions (100° C., 1200 psig, 1200 SLPH of 6% oxygen in carbon monoxide gas mixture, with stirring) were maintained for approximately 7 hours, and weight percent of diphenyl carbonate was determined by high pressure liquid chromatography over the course of the reaction. Only 1.5-2 weight % of diphenol carbonate was produced after 7 hours. A similar batch flow reaction run under the same pressure and oxygen concentration produced 17% diphenyl carbonate in 1.25 hours.

Provenance & Evidence