反应详情

Pyrinium p-toluenesulfonate (20 mg, 0.080 mmol) was added to a solution of (2R)-4-(3-fluoro-2-oxo-4-phenylpyridin-1(2H)-yl)-2-methyl-2-(methylsulfonyl)-N-(tetrahydro-2H-pyran-2-yloxy)butanamide (110 mg, 0.236 mmol) in ethanol (5 ml) and heated at reflux for 3 hours. The solution was cooled to RT, and upon cooling, a solid precipitated. The solid was collected via filtration and washed with ethanol (5 mL), heptane (10 mL), and ether (10 mL). The solid was dried under vacuum to afford the title compound as a yellow solid (38.4 mg, 42.6%). LC-MS m/z 383.0 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.60 (s, 3 H) 2.10-2.26 (m, 1 H) 3.11 (s, 3 H) 3.70-3.94 (m, 1 H) 4.07-4.30 (m, 1 H) 6.46 (t, J=6.93 Hz, 1 H) 7.46-7.57 (m, 3 H) 7.59-7.65 (m, 3 H)

1. temperatureheated
2. temperatureat reflux for 3 hours
3. temperatureupon cooling
4. customa solid precipitated
5. filtrationThe solid was collected via filtration
6. washwashed with ethanol (5 mL), heptane (10 mL), and ether (10 mL)
7. customThe solid was dried under vacuum