反应详情

HCl (1.0 N in water, 3.58 mL) was added to a solution of (2R)-4-{4-[4-(cis-3-hydroxycyclobutyl)phenyl]-2-oxopyridin-1(2H)-yl}-2-methyl-2-(methylsulfonyl)-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (620 mg, 1.20 mmol) in 1,4-dioxane (10 mL). After 2 hours the reaction was concentrated to give a brown solid. The solid was triturated with ethanol at 50° C., for 30 minutes. After cooling, filtration afforded the title compound as a white solid (384 mg, 74%). LCMS m/z 435.6 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.58 (s, 3 H) 1.83-1.98 (m, 2 H) 2.11-2.24 (m, 1 H) 2.44 (d, J=17.95 Hz, 1 H) 2.54-2.69 (m, 2 H) 2.83-3.00 (m, 1 H) 3.11 (s, 3 H) 3.65-3.84 (m, 1 H) 3.98-4.18 (m, 2 H) 6.65 (dd, J=7.02, 2.15 Hz, 1 H) 6.69 (d, J=1.95 Hz, 1 H) 7.34 (d, J=8.20 Hz, 2 H) 7.62-7.71 (m, 2 H) 7.74 (d, J=7.02 Hz, 1 H) 11.17 (br. s., 1 H)

1. concentrationAfter 2 hours the reaction was concentrated
2. customto give a brown solid
3. customThe solid was triturated with ethanol at 50° C., for 30 minutes
4. temperatureAfter cooling
5. filtrationfiltration