反应详情

To a stirred solution of 260 mg (0.88 mmol) 5-iodo-4-phenyl-pyrimidin-2-ylamine in 10 ml dioxane under argon at room temperature were added 112 mg (0.92 mmol) phenylboronic acid, 101 mg (0.09 mmol) tetrakis(triphenylphosphine)palladium(O) and 2.0 ml (4.0 mmol) 2M aqueous sodium carbonate solution. The reaction mixture was heated at reflux for 16 h, then cooled to room temperature, 1 g of kieselgel added, and the mixture concentrated in vacuo. Flash chromatography (1/1 ethyl acetate/hexane) followed by recrystallisation from ethyl acetate/pentane afforded 110 mg (51%) 2-amino-4,5-diphenylpyrimidine as a white crystalline solid. EI-MS m/e (%): 247 (M+, 90), 246 ([M—H]+, 100).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 16 h
3. addition1 g of kieselgel added
4. concentrationthe mixture concentrated in vacuo
5. customFlash chromatography (1/1 ethyl acetate/hexane) followed by recrystallisation from ethyl acetate/pentane