反应详情

温度

120 °C

To a solution of (S)-tert-butyl 2-chloro-4-(3-methylmorpholino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxylate (intermediate 4) (576 mg, 1.56 mmol) and 4-(3-ethylureido)phenylboronic acid pinacol ester (498 mg, 1.72 mmol) in DME/EtOH/H2O (12/5/3) (15 mL) was added Pd(PPh3)2(Cl)2 (55 mg, 0.078 mmol) and Na2CO3 (496 mg, 4.68 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 (20-50% EtOAc/Petroleum Ether 40-60) to yield a yellow solid (460 mg, 59%).

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 (20-50% EtOAc/Petroleum Ether 40-60)