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tetrakis(triphenylphosphine) palladium(0); In N,N-dimethyl-formamide; at 130℃;
A solution of 1-bromo-2-phenoxybenzene from step (i) above (14.8 g, 0.0594 mol), Zn(CN)2 (6.9 g, 0.0594 mol) and Pd (PPh3)4 (6.8 g, 0.00594 mol) in dimethylformamide (100 ml) was heated at 130 C. for overnight under nitrogen atmosphere. Reaction mixture was cooled to room temperature and diluted with water (200 ml). The reaction mixture was stirred with ethyl acetate (200 ml) for 15 minutes and filtered through celite. The ethyl acetate layer was separated and washed with water, brine, dried over anh. sodium sulfate and concentrated. The crude intermediate was purified by column chromatography using 4% ethyl acetate in pet ether to give the sub-title compound (10.1 g, 87.8%) as colorless liquid.
First, magnesiums (3.17 g, 120.6 mmol) areintroduced to the flask including one iodine crystal. First, 1- bromo -2-phenoxy benzenes (23.2 g, 93.2 mmol), the anhydrous tetrahydrofuran of 190 ml,and 1,2- dimethoxyethane of 26 ml and 1,2- dichloroethane of 0.78 ml areintroduced to the dropping funnel. The outbound - material blend is dipped asthe gradually. In 70 the reactant, it cools for the additional 3 hoursafter doing the mixing. Bis (3- bromophenyl) methanones (32 g, 93.2 mmol) aredissolved among THF of 200 ml and it dips as the gradually. The reactant isstirred under the reflux for 4 hours. Subsequently, the arrangement is filteredand THF is removed of the Rotavapor. The acetic acid of 400 ml and concentratedhydrochloric acid of 75 ml are added and the water of 200 ml the mixture isadded in 75for 4 hours after doing the mixing. The solid in which the colour is pale isfiltered to the suction and it washes to the methanol. Solid is stirred for1 hour among the boiling ethyl acetate and it filters and it washes to ethanol.The yield is 28.2 g (62% of the Theoretical value) as the white solid
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