反应详情

温度

80 °C

1-(2-(5-Bromo-4-(thiophen-2-yl)pyrimidin-2-ylamino)ethyl)imidazolidin-2-one (0.1 g, 0.27 mmol), 4-chlorophenylboronic acid (0.085 g, 0.54 mmol), sodium carbonate (0.27 mL of 2.0 M solution, 0.52 mmol) were added to a flask containing dioxane (1 mL). The flask was flushed with nitrogen and tetrakis(triphenylphosphine)palladium (0.062 g, 0.054 mmol) was added. The reaction was heated to 80° C. overnight. The reaction was cooled down to ambient temperature and diluted with ethyl acetate and water. The organic layer was filtered through a pad of celite and washed with saturated aqueous sodium bicarbonate, water and brine. The organic layer was then dried with sodium sulfate, concentrated and purified by column chromatography using a gradient 2 to 10% of methanol in dichloromethane to afford an off-white solid. Yield=0.04 g. MS (M+H)+ 400.

1. additionwas added
2. temperatureThe reaction was cooled down to ambient temperature
3. filtrationThe organic layer was filtered through a pad of celite
4. washwashed with saturated aqueous sodium bicarbonate, water and brine
5. dry with materialThe organic layer was then dried with sodium sulfate
6. concentrationconcentrated
7. custompurified by column chromatography
8. customto afford an off-white solid