反应详情

温度

125 °C

A mixture of 5-bromo-pyridine-2-sulfonic acid (4-fluoro-phenyl)-isobutyl-amide (150 mg, 388 μmol), 4-amino-1-methanesulfonylpiperidine (82.8 mg, 465 μmol), Pd2(dba)3 (36 mg, 39 μmol), XantPhos (22 mg, 39 μmol), and sodium tert-butoxide (82 mg, 853 μmol) in toluene (4 mL) was degassed with nitrogen then heated at 125° C. for 30 minutes in a microwave reactor. Saturated aqueous NaHCO3 was added and then extracted with EtOAc, washed with brine, concentrated and purified by silica gel column chromatography (0-75% EtOAc in cyclohexane) to give the title compound (103 mg). 1H NMR (400 MHz, DMSO-d6): δ 8.10 (d, 1H), 7.36 (d, 1H), 7.15 (d, 4H), 6.96 (dd, 1H), 6.81 (d, 1H), 3.50-3.52 (m, 5H), 2.89 (s, 5H), 1.99 (s, 2H), 1.43-1.47 (m, 3H), 0.83 (d, 6H). LCMS (m/z, Method A) ES+ 484.9 [M+1]+.

1. customwas degassed with nitrogen
2. additionSaturated aqueous NaHCO3 was added
3. extractionextracted with EtOAc
4. washwashed with brine
5. concentrationconcentrated
6. custompurified by silica gel column chromatography (0-75% EtOAc in cyclohexane)