反应详情

温度

150 °C

4-Bromo-2-chloropyridine (125 mg, 0.65 mmol), isobutyl piperazine-1-carboxylate (93 mg, 0.5 mmol), Pd2(dba)3 (10 mg, 10 μmol), t-BuONa (72 mg, 0.75 mmol), and Xantphos (17 mg, 30 μmol) in dry toluene (5 mL) were sealed in a microwave vessel and heated by microwave irradiation at 150° C. for 15 minutes. The reaction was diluted with EtOAc, washed with water, dried over Na2SO4, and evaporated under reduced pressure. Purification by flash chromatography (SiO2, MeOH/CH2Cl2) afforded 3a as a tan oil (94 mg, 63% yield). LCMS: m/z 298.5 (M+H)+ at 1.93 minutes (10%-99% CH3CN/H2O), (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA).

1. washwashed with water
2. dry with materialdried over Na2SO4
3. customevaporated under reduced pressure
4. customPurification by flash chromatography (SiO2, MeOH/CH2Cl2)