反应详情

温度

40 °C

A mixture of 4-6 (3.94 g, 7.43 mmol), trifluoroacetic acid (30.0 mL, 392 mmol), and dichloromethane (30.0 mL) was stirred at 40° C. for 19 hours under an atmosphere of nitrogen gas and concentrated under reduced pressure. To the resulting residue was added saturated aqueous NaHCO3 (300 mL) and hexane/dichloromethane (5:1) (150 mL) at ambient temperature. The resulting mixture was stirred vigorously at ambient temperature for 30 minutes. The precipitated solid was filtered, washed with water (60 mL) and hexane/dichloromethane (5:1) (60 mL), and dried under high vacuum to give 2.08 g (96%) of 4-7 as a pale yellow solid: 1H NMR (400 MHz, DMSO-d6) δ 9.04 (1H, br s), 8.28 (1H, d, J=6.0 Hz), 8.05 (2H, m), 7.97 (2H, m), 7.55 (1H, br d, J=6.0 Hz), 6.78 (2H, br s), 6.63 (1H, br s); ESI-MS m/z 291 [C16H10N4O2+H]+.

1. concentrationconcentrated under reduced pressure
2. additionTo the resulting residue was added saturated aqueous NaHCO3 (300 mL) and hexane/dichloromethane (5:1) (150 mL) at ambient temperature
3. stirringThe resulting mixture was stirred vigorously at ambient temperature for 30 minutes
4. filtrationThe precipitated solid was filtered
5. washwashed with water (60 mL) and hexane/dichloromethane (5:1) (60 mL)
6. customdried under high vacuum