反应详情

温度

120 °C

To a solution of 2-(benzyloxy)-5-bromopyridine (1.5 g, 5.6 mmol), piperidin-4-yl 4-isopropylpiperazine-1-carboxylate (2.15 g, 8.4 mmol) in toluene (30 mL) was added Pd2(dba)3 (1.57 g, 2.2 mmol), BINAP (2.79 g, 4.4 mmol) and t-BuOK (3.78 g, 33.8 mmol). The reaction was stirred under the microwave irradiation at 120° C. for 20 min. The mixture was diluted with EA (100 mL) and washed with water (3×50 mL). The organic phase was separated, dried and concentrated to dryness. The residue was taken into dilute HCl (pH=1, 100 mL) and the mixture was extracted with DCM (3×100 mL) to remove impurities. The aqueous phase was made basic (pH=9-10) with solid Na2CO3 and extracted with DCM (3×100 mL). The combined organic layers were dried, concentrated and purified by silica gel chromatography (EA/MeOH=50/1) to give the title compound as a white solid (500 mg, 20%). [LCMS: Rt=2.09 mim, m/z 439.3 (M+H)+].

1. washwashed with water (3×50 mL)
2. customThe organic phase was separated
3. customdried
4. concentrationconcentrated to dryness
5. extractionthe mixture was extracted with DCM (3×100 mL)
6. customto remove impurities
7. extractionextracted with DCM (3×100 mL)
8. customThe combined organic layers were dried
9. concentrationconcentrated
10. custompurified by silica gel chromatography (EA/MeOH=50/1)