反应详情

To a solution of 3 (1 g, 3.32 mmol) in THF (5 mL) was added methylamine (10.5 mL of 40% water solution). The solution was stirred for 30 min and then extracted with EtOAc (30 mL). The organic phase was washed with DI water (2×20 mL), dried and concentrated to give a red oil. Purification by chromatography (MeOH/DCM 1:99) yielded yellow solid.(0.8 g, 96%) 1H NMR (400 MHz CDCl3) δ8.09 (1H, d, J=8.4 Hz), 8.02 (1H, d, J=7.2 Hz), 7.77 (1H, d, J=8 Hz), 7.49 (1H, d, J=8.4 Hz), 7.36 (1H, t, J=8.0 Hz), 4.12 (2H, s), 2.58 (3H, s).

1. extractionextracted with EtOAc (30 mL)
2. washThe organic phase was washed with DI water (2×20 mL)
3. customdried
4. concentrationconcentrated
5. customto give a red oil
6. customPurification by chromatography (MeOH/DCM 1:99)
7. customyielded yellow solid