反应详情

温度

50 °C

A suspension of the product of Example 34, Step D (0.07 g; 0.118 mmol), MnO2 (0.58 g; 6.67 mmol) and anhydrous MgSO4 (0.5 g; 4.2 mmol) in 1,2-dichloroethane (2.5 ml) was vigorously stirred for 2 h at ˜50° C., then overnight at room temperature. This was diluted to 20 ml with CH2Cl2 and filtered through Celite pad, washed with fresh CH2Cl2 (10 ml). The combined organic phase was evaporated under reduced pressure and the residue was purified by FCC (SiO2, CH2Cl2/EtOAc 9:1) to give the title compound (0.02 g; 28%), as creamy solid. 1H-NMR (CDCl3) 1.43-1.53 (m, 21H+H2O); 3.78 (d, 2H, J=11.9 Hz); 3.90 (d, 2H, J=11.9 Hz); 4.13-4.38 (m, 5H); 4.76 (s, 1H); 6.98 (d, 1H, J=8.5 Hz); 7.15 (s, 1H); 7.28-7.34 (m, 2H); 7.68 (d, 1H, J=8.4 Hz); 7.73 (d, 1H, J=1.9 Hz); 7.83 (dd, 1H, J=1.9, 8.4 Hz); 8.03 (d, 1H, J=7.2 Hz).

1. customovernight
2. customat room temperature
3. filtrationfiltered through Celite pad
4. washwashed with fresh CH2Cl2 (10 ml)
5. customThe combined organic phase was evaporated under reduced pressure
6. customthe residue was purified by FCC (SiO2, CH2Cl2/EtOAc 9:1)