反应详情

温度

50 °C

A solution of the product from Example 1G (5 g, 13.44 mmol) in DCM (80 mL) and MeOH (40 mL) was treated with hydrogen peroxide (5.2 mL, 30% in H2O, 53.8 mmol). The mixture was heated to 50° C. for 48 hours. The mixture was concentrated under reduced pressure to a smaller volume while still in a solution. The solution was loaded onto an ANALOGIX SuperFlash silica gel column (ANALOGIX is a registered trademark of Analogix Inc. of Burlington, Wis.) and eluted with NH4OH /MeOH/DCM (1/10/90) to obtain the slower moving component (comparing with Example 1H) as the title product. 1H NMR (300 MHz, DMSO) δ ppm 8.07 (m, 1 H), 7.70 (d, J=9 Hz, 2 H), 7.57 (d, J=9 Hz, 4 H), 7.50 (d, J=6 Hz, 1 H), 7.08 (dd, dd, J=9, 4.0 Hz, 1 H), 6.65 (d, J=9 Hz, 2 H), 4.48-4.54 (m, 1 H), 3.81-3.87 (m, 1 H), 3.66-3.74 (m, 2 H), 3.36-3.42 (m, 2 H), 3.24 (m, 1 H), 3.09 (s, 3 H), 2.11-2.17 (m, 1 H); MS (DCI,) M+=388.

1. concentrationThe mixture was concentrated under reduced pressure to a smaller volume while still in a solution
2. wash) and eluted with NH4OH /MeOH/DCM (1/10/90)
3. customto obtain the