反应详情

Into a solution of 2 (1.25 g, 3.61 mmol) in CHCl3 (25 mL) was added 5 (0.66 g, 3.61 mmol), EEDQ (1.07 g, 4.32 mmol), and triethylamine (0.74 mL, 5.33 mmol). The solution was stirred at reflux for 19 h before cooling to RT and adding EtOAc. The solution was washed sequentially with 1N HCl, 0.1N NaOH, water, and brine, before drying over MgSO4 and concentrating under reduced pressure. The crude material was purified on a silica gel column eluted with 20% moving to 50% EtOAc in hexanes. Combined and concentrated pure fractions to give 6 (0.33 g, 18%). MS: APCI (AP+): 510.3 (M)+, (AP−): 508.4 (M)−.

1. temperatureat reflux for 19 h
2. washThe solution was washed sequentially with 1N HCl, 0.1N NaOH, water, and brine
3. dry with materialbefore drying over MgSO4
4. concentrationconcentrating under reduced pressure
5. customThe crude material was purified on a silica gel column
6. washeluted with 20%
7. concentrationconcentrated pure fractions