反应详情

HCl (4.0 M in 1,4-dioxane, 1.0 mL) was added to a solution of 4-[4-{4-[3-(4,4-difluoropiperidin-1-yl)propoxy]phenyl}-2-oxopyridin-1(2H)-yl]-2-methyl-2-(methylsulfonyl)-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (209 mg, 0.334 mmol) in 1,4-dioxane/water (1:1, 5 mL). After 10 minutes the reaction was concentrated to give a white solid, the solid was triturated with 2-propanol at 50° C. for 1 h. The title compound was isolated by filtration as a white solid (146 mg, the hydrochloride salt, 75%). LCMS m/z 542.8 (M+1) 1H NMR (400 MHz, DMSO-d6) δ ppm 1.57 (s, 3 H) 2.22 (br. s., 3 H) 2.38 (br. s., 5 H) 3.11 (s, 3 H) 3.13-3.26 (m, 2 H) 3.31 (br. s., 2 H) 3.74 (br. s., 3 H) 4.14 (t, J=5.76 Hz, 3 H) 6.59-6.72 (m, 2 H) 7.05 (d, J=8.78 Hz, 2 H) 7.63-7.79 (m, 3 H) 11.03 (br. s., 1 H) 11.18 (br. s., 1 H)

1. concentrationAfter 10 minutes the reaction was concentrated
2. customto give a white solid
3. customthe solid was triturated with 2-propanol at 50° C. for 1 h