反应详情

To 2,4-Dimethoxypyrimidine-5-boronic acid (200 mg, 10.6 mmol), Iodobenzene (326 mg, 1.60 mmol) and K3PO4 (900 mg, 4.24 mmol) in DMSO (5 mL, purged with Ar) was added 1,1′bis(diphenylphosphino)ferrocene palladium chloride, complex with dichloromethane (12 mg) and the reaction solution was heated to 60 C in a sealed tube. The solution was heated for 2 h, stirred at room temperature for 10 hr and filtered through celite. The solution was poured into sat. NaHCO3 to give a gray solid. This material was collected, dissolved in ethyl acetate, dried (Na2SO4). Flash chromatography 0 to 2% methanol in dichloromethane gave 2,4-Dimethoxy-5-phenyl-pyrimidine (171 mg, 75% yield). HPLC tr=5.62 min (83%), FIA m/e 217.2 (M+H), HNMR (500 MHz, CDCl3); δ8.25 (1H, s), 7.45–7.29 (5H, m), 4.00 (3H, s), 3.98 (3H, s).

1. temperaturethe reaction solution was heated to 60 C in a sealed tube
2. temperatureThe solution was heated for 2 h
3. filtrationfiltered through celite
4. additionThe solution was poured into sat. NaHCO3
5. customto give a gray solid
6. customThis material was collected
7. dissolutiondissolved in ethyl acetate
8. dry with materialdried (Na2SO4)