反应详情

To a solution of compound 55 (318 mg, 1.56 mmol) in DMF (1 mL) was added dropwise CbzCl (0.29 mL, 2.03 mmol) at 0° C. with stirring. The reaction mixture was stirred at room temperature for 3 h. The DMF was removed by vacuum. The residue was purified with silica gel column chromatography (EtOAc:CH3OH:TEA=3:1:0.2) to give compound 56 (400 mg, 76%) as a light yellow oil. 1H NMR (400 MHz, CDCl3) δ7.70 (s, 1H), 7.30-7.40 (m, 5H), 7.25 (d, 2H, J=8.3 Hz), 6.98 (d, 2H, J=8.3 Hz), 5.15 (s, 2H), 3.65 (s, 4H), 2.50 (t, 2H, J=7.4 Hz), 2.43 (d, 2H, J=7.4 Hz), 1.85-1.97 (m, 2H).

1. stirringThe reaction mixture was stirred at room temperature for 3 h
2. customThe DMF was removed by vacuum
3. customThe residue was purified with silica gel column chromatography (EtOAc:CH3OH:TEA=3:1:0.2)