反应详情

温度

70 °C

N-[2-(6-Amino-pyridine-2-carbonyl)-5-chloro-pyridin-3-yl]-4-tert-butyl-benzenesulfonamide (52 mg, 0.1 mmol) in pyridine was treated with methanesulfonyl chloride (100 mg) and then stirred at 70° C. for 2 h. After evaporation of solvent under reduced pressure, to the mixture was added THF (5 mL), followed by NaOH (2 N, 2 mL) and stirred at room temperature for another 2 h. The mixture was dissolved in EtOAc and washed with 1 N HCl, NaHCO3 (saturated), brine, dried over MgSO4, concentrated under reduced pressure, and purified through automated normal-phase chromatography to afford the title compound: 1H NMR (400 MHz, CDCl3) δ 11.0 (s, 1 H), 8.37 (d, 1 H), 8.25 (d, 1 H), 7.82 (d, 2H), 7.72 (m, 1 H), 7.61 (d, 1 H), 7.42 (d, 2H), 7.17 (d, 1 H), 3.15 (s, 3H), 1.23 (s, 9H); MS (ES) (M+H)+ expected 523.1, found 523.1.

1. customAfter evaporation of solvent under reduced pressure
2. additionto the mixture was added THF (5 mL)
3. stirringstirred at room temperature for another 2 h
4. dissolutionThe mixture was dissolved in EtOAc
5. washwashed with 1 N HCl, NaHCO3 (saturated), brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated under reduced pressure
8. custompurified