反应详情

温度

30 °C

Potassium carbonate (5.73 g, 41.57 mmol, 3.0 eq), Pd2(dba)3 (1.26 g, 1.39 mmol, 0.1 eq) and tri-tert-butyl phosphonium tetrafluoroborate (0.2 g, 0.69 mmol, 0.05 eq) were added at room temperature under an argon atmosphere to a stirred solution of (1-(5-bromopyrimidin-2-yl)-3-(methylthio)-1H-indol-6-yl)(morpholino)-methanone (6.0 g, 13.85 mmol, 1.0 eq) and (2-fluorophenyl)boronic acid (2.31 g, 16.62 mmol, 1.2 eq) in THF/water (100 mL, 4:1). The mixture was stirred for 2 h at 30° C., diluted with ethyl acetate (50 mL), and filtered through a pad of celite. The filtrate was washed with water, dried over sodium sulphate and evaporated. The residue was purified by column chromatography [100-200 mesh; ethyl acetate/petrolether=2:3]. Yield: 4.0 g (64% of theory).

1. filtrationfiltered through a pad of celite
2. washThe filtrate was washed with water
3. dry with materialdried over sodium sulphate
4. customevaporated
5. customThe residue was purified by column chromatography [100-200 mesh; ethyl acetate/petrolether=2:3]