反应详情

3-Chloro-5-methyl-2H-isoquinolin-1-one (50 mg, 0.26 mmol), 2-(4-methylpiperazin-1-yl)pyrimidine-5-boronic acid pinacol ester (118 mg, 0.39 mmol), K2CO3 (73 mg, 0.52 mmol) and Pd(dppf)Cl2 (10 mg, 0.013 mmol) in DME/EtOH/H2O 4:0.5:1 (2.75 mL) were added to a microwave vial and the reaction mixture purged with N2 for 10 min. The reaction mixture was irradiated using a microwave reactor (300 W, 100° C., 60 min). The reaction mixture was filtered through celite and concentrated in vacuo. The crude material was purified by silica gel column chromatography, eluting with CH2Cl2 and increasing the polarity to 50% MeOH/CH2Cl2. The crude material was trituared with MeOH and washed with isohexane to afford 5-methyl-3-[2-(4-methyl-piperazin-1-yl)-pyrimidin-5-yl]-2H-isoquinolin-1-one as an off-white solid (28 mg, 32%).

1. customthe reaction mixture purged with N2 for 10 min
2. customThe reaction mixture was irradiated
3. custom(300 W, 100° C., 60 min)
4. filtrationThe reaction mixture was filtered through celite and
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by silica gel column chromatography
7. washeluting with CH2Cl2
8. temperatureincreasing the polarity to 50% MeOH/CH2Cl2
9. washwashed with isohexane