反应详情

温度

70 °C

Pyridinium p-toluenesulfonate (360 mg, 0.50 mmol) was added to a solution of (2R)-4-{5-fluoro-2-oxo-4-[4-(2H-1,2,3-triazol-2-yl)phenyl]pyridin-1(2H)-yl}-2-methyl-2-(methylsulfonyl)-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (1.53 g, 2.87 mmol) in ethanol (60 mL). The solution was heated to 70° C. and was stirred at this temperature for 3 h. The reaction was allowed to cool and was stirred at rt for three days. The solid was collected via filtration, washed with ethanol (20 mL) and hexanes (20 mL). The solid was dried under vacuum to afford the title compound as a white solid (1.05 g, 81.5%). MS (LCMS) m/z 450.0 (M+1), 1H NMR (400 MHz, DMSO-d6) δ ppm 1.58 (s, 3H) 2.08-2.27 (m, 0H) 2.38-2.59 (m, 1H) 3.12 (s, 3H) 3.72-3.90 (m, 1H) 4.00-4.17 (m, 1H) 6.62 (d, J=7.61 Hz, 1H) 7.70-7.88 (m, 2H) 8.08 (d, J=6.63 Hz, 1H) 8.12-8.18 (m, 2H) 8.19 (s, 2H) 9.25 (d, J=1.95 Hz, 1H) 11.09 (d, J=1.76 Hz, 1H).

1. temperatureto cool
2. stirringwas stirred at rt for three days
3. filtrationThe solid was collected via filtration
4. washwashed with ethanol (20 mL) and hexanes (20 mL)
5. customThe solid was dried under vacuum