反应详情

温度

100 °C

A solution of C9 (0.253 mmol) and anhydrous DMSO (0.5 ml) was treated with 1-(4-aminophenyl)ethanol (0.277 mmol) followed by potassium phosphate dibasic (0.746 mmol). The mixture was stirred at 100° C. for 1.5 days, and treated with additional 1-(4-aminophenyl)ethanol (0.583 mmol). The mixture was stirred at 100° C. for 15 hours and concentrated. The resultant residue was purified first by column chromatography (silica gel; 10% (NH4OH/MeOH)/CH2Cl2) followed by preparatory thin layer chromatography developed in 5% MeOH/CH2C12 to provide 12. Yield: 13.6 mg, 10.8%. 1H NMR (CD3OD) δ: 8.39 (d, 1H), 8.13 (s, 1H), 7.73 (d, 1H), 7.33 (m, 3H), 7.14 (d, 2H), 4.87 (s, 2H), 4.72 (q, 1H), 3.17 (s, 3H), 3.10 (s, 3H), 1.37 (d, 3H). MS: m/z 497 (MH+).

1. stirringThe mixture was stirred at 100° C. for 15 hours
2. concentrationconcentrated
3. customThe resultant residue was purified first by column chromatography (silica gel; 10% (NH4OH/MeOH)/CH2Cl2)