反应详情

温度

60 °C

A mixture of [5-(benzyloxy)-1-methyl-6-oxo-1,6-dihydropyridin-3-yl]boronic acid (30 mg, 0.116 mmol), 2-chloro-4-phenylpyrimidine (23.2 mg, 0.122 mmol), bis(tri-t-butylphosphine)palladium(0) (5.9 mg, 0.012 mmol) and potassium fluoride (24 mg, 0.405 mmol) in dioxane (1.5 mL) was stirred at 60° C. for 22 h, cooled to room temperature and filtered through a plug of silica gel (washed with EtOAc). Combined filtrate and washings were concentrated. Purification by preparative HPLC (5-55% CH3CN/H2O over 20 min, 0.05% added TFA) afforded 21 mg 3-(benzyloxy)-1-methyl-5-(4-phenylpyrimidin-2-yl)pyridin-2(1H)-one (49%) as a yellow solid. LC/MS (M+H)+ 370.3.

1. temperaturecooled to room temperature
2. filtrationfiltered through a plug of silica gel (washed with EtOAc)
3. concentrationCombined filtrate and washings were concentrated
4. customPurification
5. additionby preparative HPLC (5-55% CH3CN/H2O over 20 min, 0.05% added TFA)