反应详情

To a solution of (2R)-2-methyl-2-(methylsulfonyl)-4-{2-oxo-4-[4-(tetrahydro-2H-pyran-4-yl)phenyl]pyridin-1(2H)-yl}-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (82 mg, 0.15 mmol) in 2-propanol (1.5 mL) was added 1.0 N hydrochloric acid (0.77 mL). The solution was stirred for 1 h. The reaction was concentrated, the residue was triturated with 2-propanol as a white suspension at 50° C. for 30 minutes. A white solid was collected by filtration (75%). LCMS m/z 449.0 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.57 (s, 3 H) 1.65-1.74 (m, 4 H) 2.11-2.21 (m, 1 H) 2.37-2.47 (m, 1 H) 2.83 (tt, J=10.40, 5.42 Hz, 1 H) 3.11 (s, 3 H) 3.39-3.49 (m, 2 H) 3.74 (td, J=12.01, 4.69 Hz, 1 H) 3.92-3.99 (m, 2 H) 4.11 (td, J=11.91, 5.08 Hz, 1 H) 6.65 (dd, J=7.03, 2.15 Hz, 1 H) 6.69 (d, J=2.15 Hz, 1 H) 7.37 (m, 2 H) 7.67 (m, 2 H) 7.74 (d, J=7.23 Hz, 1 H) 9.27 (br. s., 1 H) 11.19 (s, 1 H).

1. concentrationThe reaction was concentrated
2. customthe residue was triturated with 2-propanol as a white suspension at 50° C. for 30 minutes
3. filtrationA white solid was collected by filtration (75%)