反应详情

温度

100 °C

The product from Example 1B (0.54 g, 2.16 mmol) and the product from Example 1C (0.50 g, 2.14 mmol) in isopropanol (5 mL) were placed in a sealed tube and heated at 100° C. for 18 hours. The mixture was concentrated and the residue was purified by column chromatography on silica gel (24:1 CHCl3:methanol) to provide the title compound as a colorless solid (0.44 g, 42%). Rf=0.55 (CHCl3:methanol, 9:1); 1H NMR (CDCl3) δ 7.30-7.14 (m, 10H), 4.61 (br s, 2H), 3.87 (m, 2H), 2.87-2.77 (m, 2H), 2.72 (dd, J=7.4, 13.6 Hz, 2H), 2.57 (d, J=5.8 Hz, 4H), 1.41 (s, 18H); MS (APCl+) m/z 484 (M+H)+.

1. concentrationThe mixture was concentrated
2. customthe residue was purified by column chromatography on silica gel (24:1 CHCl3:methanol)