反应详情

温度

80 °C

5-(Benzyloxy)-1-(biphenyl-3-yl)-4-oxo-1,4-dihydropyridine-2-carboxylic acid (48.0 g, 121 mmol), DIPEA (31.25 g, 242 mmol), and DPPA (49.9 g, 91.2 mmol) were added to t-BuOH (500 mL) at room temperature. The resulting solution was heated to at 80° C. for 16 h. After cooling to room temperature, the mixture was concentrated to give a residue which was purified by silica gel chromatography to afford tert-butyl[5-(benzyloxy)-1-(biphenyl-3-yl)-4-oxo-1,4-dihydropyridin-2-yl]carbamate. !H NMR δ (400 MHz, CDCl3): 7.70 (d, J−7.6 Hz, 1H), 7.58-7.53 (m, 3H), 7.47 (m, 2H), 7.42-7.37 (m, 4H), 7.33-7.20 (m, 3H)1 7.18 (d, J=7.2 Hz, 1H), 6.94 (s, 1H), 6.87 (s, 1H), 6.09 (s, 1H), 5.12 (s, 2H)f 1.34 (s, 9H). MS (ESI) (M+H)+ 469.

1. temperatureAfter cooling to room temperature
2. concentrationthe mixture was concentrated
3. customto give a residue which
4. customwas purified by silica gel chromatography