Benzoic Acid → HCID 59412516, compound

Participants

Reaction Steps

913 mg (3 mmol) of tri-o-tolylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a well-stirred suspension of 22.5 g (40 mmol) of the resultant 9-bromo-10-(7-bromobenz[a]anthracen-4-yl)-anthracene, 12.2 g (100 mmol) of benzoic acid, 25.5 g (120 mmol) of tripotassium phosphate in a mixture of 300 ml of toluene, 100 ml of dioxane and 400 ml of water, and the mixture is subsequently heated under reflux for 16 h. After cooling, the precipitated solid is filtered off with suction, washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v), three times with 100 ml of ethanol and finally dried. Recrystallisation five times from DMF (about 3 ml/g); sublimation (p=5×10−5 mbar, T=350° C.). Yield: 12.6 g (23 mmol), 46.0%, purity 99.9% (HPLC), Tg=171.8° C.

Provenance & Evidence