反应详情

温度

80 °C

To a solution of 6-Acetyl-2H-benzo[b][1,4]oxazin-3(4H)-one (14) (0.5 mmol) in TFA (4 mL) was added Et3SiH (1.0 mmol). The reaction was heated at 80° C. for 2 h and then concentrated in vacuo. The residue was treated with sat aqueous NaHCO3 and the resulting solid was isolated by filtration, washed with water and dried in vacuo to give a white solid: 1H NMR (DMSO-d6, 400 MHz): δ=10.63 (s, 1H), 6.81-6.87 (m, 1H), 6.71 (s, 1H), 6.74 (d, J=8.1 Hz, 1H), 4.51 (s, 2H), 2.46-2.54 (m, 2H), 1.12 ppm (t, J=7.6 Hz, 3H). ESI-MS: m/z 178.0 (M+H)+.

1. concentrationconcentrated in vacuo
2. additionThe residue was treated with sat aqueous NaHCO3
3. customthe resulting solid was isolated by filtration
4. washwashed with water
5. customdried in vacuo
6. customto give a white solid