反应详情

温度

190 °C

MgSO4 (1.41 g, 11.78 mmol) was added to a suspension of 436 (1.16 g, 3.93 mmol), 2-fluoro-4-nitrophenol (1.23 g, 7.85 mmol) and Na2CO3 (1.24 g, 11.78 mmol) in Ph2O (10 mL). The suspension was heated at 160° C. for 1.5 h and at 190° C. for 2 h. After cooling to room temperature, DCM (30 mL) was added and the reaction mixture was filtered and concentrated. The residue was purified by biotage (SNAP 25 g cartridge; AcOEt/Hexane:10/90 over 5 CV then MeOH/DCM: 0/100 to 10/90 over 20CV), to afford the title compound 437 (1.20 g, 2.88 mmol, 73% yield) as a yellow solid. MS (m/z): 417.2 (M+H).

1. temperatureAfter cooling to room temperature
2. filtrationthe reaction mixture was filtered
3. concentrationconcentrated
4. customThe residue was purified by biotage (SNAP 25 g cartridge