反应详情

To a solution of 1A (1.44 g, 9.0 mmol) in toluene (24 ml) was added POCl3 (13.5 ml) and DEA (3.6 ml). The mixture was refluxed under N2 for 30 min. After cooling to room temperature, the reaction mixture was concentrated under vacuum. The residue was dissolved in EtOAc, washed with 10% citric acid solution, followed by saturated NaHCO3. The residue was dried with MgSO4, filtered, and concentrated to give 1B (1.37 g, 85%) as a solid. 1H-NMR (400 MHz, CDCl3): 8.96 (s, 1H), 7.94 (d, J=8.52 Hz, 1H), 7.80 (dd, J=7.17 Hz, J=8.52 Hz, 1H), 7.51 (d, J=7.17 Hz, 1H), 3.05 (s, 3H).

1. temperatureThe mixture was refluxed under N2 for 30 min
2. concentrationthe reaction mixture was concentrated under vacuum
3. dissolutionThe residue was dissolved in EtOAc
4. washwashed with 10% citric acid solution
5. dry with materialThe residue was dried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated