反应详情

温度

130 °C

A vial is charged with methyl 5-aminopicolinate 2 (0.83 mmol), 2-chloro-5-(4-methoxy-phenyl)-pyrimidine 3 (0.83 mmol), Pd(OAc)2 (0.124 mmol), xanthphos (0.124 mmol), Cs2CO3 (0.83 mmol) and anhydrous 1,4-dioxane (5 mL). The vial is evacuated and refilled with N2 twice and the mixture is heated in a microwave oven at 130° C. for 20 min. The vial is cooled to it and the reaction mixture is diluted with DCM, washed with 10% NH4Cl solution, brine and dried over Na2SO4. The solvent is removed in vacuum and the crude is triturated with EtOAc to afford 5-[5-(4-methoxy-phenyl)-pyrimidin-2-ylamino]-pyridine-2-carboxylic acid methyl ester 4 as light brown solid. NMR (400 MHz, d6-DMSO) δ 10.62 (s, 1H), 8.93 (s, 2H), 8.83 (bs, 1H), 8.46 (d, J=8.0 Hz, 1H), 8.27 (d, J=8.0 Hz, 1H), 7.72-7.70 (m, 2H), 7.08-7.06 (m, 2H), 3.86 (s, 3H), 3.81 (s, 3H). MS (m/z) (M+1)+: 337.1.

1. customThe vial is evacuated
2. additionrefilled with N2 twice
3. temperatureThe vial is cooled to it
4. additionthe reaction mixture is diluted with DCM
5. washwashed with 10% NH4Cl solution, brine
6. dry with materialdried over Na2SO4
7. customThe solvent is removed in vacuum
8. customthe crude is triturated with EtOAc