HCID 21951478, compound → HCID 21951486, compound

Participants

Reaction Steps

Into a 250 mL Paar Hydrogenation flask was charged [2,5-bis(4-nitrophenoxy)phenyl]diphenylphosphine oxide (5.4 g, 0.0098 mol) and 1,4-dioxane (100 mL). The solution was warmed to effect dissolution with subsequent cooling to room temperature upon which 10% Pd/C (0.59 g) was added. The mixture was degassed prior to the introduction of hydrogen gas. The mixture was agitated under a hydrogen atmosphere for ˜24 hours at room temperature. After degassing the solution, the Pd/C was removed by filtration and the solution added to stirred water to afford an off white solid. The crude solid was collected via filtration, washed with water, and dried at room temperature to afford 4.1 g (76% crude yield). The solid exhibited a broad endothermic peak at 200.7° C. as determined by DSC at a heating rate of 10° C./min. Recrystallization from aqueous ethanol afforded a tan solid (3.2 g, 80% yield) exhibiting a broad endothermic peak at 204.12° C. by DSC.

Provenance & Evidence