反应详情

温度

120 °C

Step B To a solution of 3-methoxy-4-nitrophenol (0.5 g, 3 mmol) prepared in Example 132 Step A in anhydrous DMF (13 mL) were added Cs2CO3 (2.9 g, 8.9 mmol) and methanesulfonic acid tetrahydropyran-4-yl ester (0.64 g, 3.6 mmol) sequentially. The reaction mixture was heated at 120° C. for 3 h. The mixture was cooled to room temperature, and diluted with water. The mixture was extracted with ethyl acetate three times. The combined organic extract was washed with water, brine, dried over MgSO4, and concentrated. The residue was purified by chromatography (40-60% EtOAc in hexanes) to give 4-(3-methoxy-4-nitrophenoxy)tetrahydro-2H-pyran as a yellow oil (0.4 g, 53%).

1. temperatureThe mixture was cooled to room temperature
2. extractionThe mixture was extracted with ethyl acetate three times
3. extractionThe combined organic extract
4. washwas washed with water, brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe residue was purified by chromatography (40-60% EtOAc in hexanes)