Synthesis
A solution of 10.0 g of 2-bromobiphenyl (42.9 mmol) in 70 ml of anhydrous THF was added to a 500 mE 3-neck flask and cooled to -78 C. 27 ml of a 1.58 M hexane solution of n-BuEi (42.9 mmol) was then added dropwise while stirring, and the reaction was stirred for about 2.5 hours. A solution of 9.30 g (35.6 mmol) of 3-bromobenzophenone in 85 mE of an anhydrous THF was added dropwise, and the resulting mixture was stirred for about 2 hours at -78 C. followed by stirring for about 3 hours at room temperature. 1 N hydrochloric acid (HC1) was then added to the mixture and stirred for about 1 hour. The mixture was washed with water, and the resultant organic phase was concentrated to afford a material having a candy-like consistency. The candy-like material, 50 ml of acetic acid, and 2.4 ml of hydrochloric acid were added to a 500 mL recovery flask, and the mixture was stirred and reacted at 130 C. under a nitrogen atmosphere for about 2 hours. After the reaction, the reaction mixture was added dropwise to 350 ml of ice-cold water, precipitating white crystals, and the crystals were isolated by filtration. The crystals were washed with methanol and allowed to dry. About 13.3 g of Compound A was obtained as a white powder (yield: about 78%).
