反应详情

温度

80 °C

To a stirred solution of 27 (2.90 g, 6.09 mmol) in anhydrous DMF (11 mL) were added K2CO3 (2.53 g, 18.3 mmol) and 4-nitrophenol (0.847 g, 6.09 mmol), and the reaction mixture was heated to 80° C. for 16 h. After cooling, the reaction mixture was diluted in water, extracted three times with CH2Cl2, and then dried over MgSO4. The filtrate was concentrated under reduced pressure to give 28 as an oily residue (2.65 g, 98%): 1H NMR (300 MHz, CDCl3) δ 8.18 (d, J=9.2 Hz, 2H), 6.99 (d, J=9.2 Hz, 2H), 4.69-4.56 (m, 1H), 4.28-4.17 (m, 2H), 3.97-3.42 (m, 18H), 1.95-1.41 (m, 6H). 13C NMR (75 MHz, CDCl3) δ 163.82, 141.40, 125.75, 114.52, 98.83, 70.81, 70.51, 70.43, 69.27, 68.15, 66.54, 62.12, 30.48, 25.34, 19.41.

1. temperatureAfter cooling
2. extractionextracted three times with CH2Cl2
3. dry with materialdried over MgSO4
4. concentrationThe filtrate was concentrated under reduced pressure