1-Bromo-4-(methylsulphonyl)benzene → 1-(6-Methylpyridin-3-yl)-2-(4-(methylsulfonyl)phenyl)ethanone

Participants

Reaction Conditions

Reaction Steps

To a four-neck round-bottom 250 ml flask equipped with mechanical stirring and condenser were added at 20-25° C. and under nitrogen atmosphere Xantphos, palladium acetate, tripotassium phosphate trihydrate, PVP, 4-bromophenyl methyl sulfone, 5-acetyl-2-methyl pyridine, water (50.00 ml). A vacuum/nitrogen cycle was repeated for at least three times at 20-25° C. The resulting reaction mixture was heated up to 85-90° C. and stirred for at least 24 h. The reaction mixture was transferred in an other recipient then cooled down to 40-50° C. and diluted with water (400 ml). The resulting mixture was stirred at 40-45° C. for 15 min and cooled down to −5-0° C. The resulting reaction mixture was stirred at −5-0° C. for at least 2 h, then it was filtered and the cake was washed with water (3×100 ml) and dried at 65-70° C. under reduced pressure to afford a crude product of formula (I) as a yellow solid (48.3 g). yield: 90.1%, Purity: 75.7% by HPLC A %.

Provenance & Evidence