反应详情

温度

120 °C

To a solution of (S)-4-(2-chloropyrimidin-4-yl)-3-methylmorpholine (Intermediate 3) (100 mg, 0.47 mmol) and 4-(3-ethylureido)phenylboronic acid pinacol ester (143 mg, 0.52 mmol) in DME:EtOH:H2O (12:5:3, 2 mL) was added Pd(PPh3)2(Cl)2 (17 mg, 0.024 mmol) and Na2CO3 (149 mg, 1.41 mmol). The reaction mixture was then heated by microwave at 120° C. for 1 h. The crude reaction mixture was then partitioned between water and EtOAc, the phases separated and the organic layer washed with aqueous NaHCO3 and brine, dried over magnesium sulfate, filtered and the solvent removed in vacuo. The residue was purified by flash chromatography (2-5% MeOH/DCM) to yield a white solid (12 mg, 8%).

1. customThe crude reaction mixture
2. customwas then partitioned between water and EtOAc
3. customthe phases separated
4. washthe organic layer washed with aqueous NaHCO3 and brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent removed in vacuo
8. customThe residue was purified by flash chromatography (2-5% MeOH/DCM)