反应详情

To a solution of 4′-fluoro-5-(methoxycarbonyl)biphenyl-3-carboxylic acid (400 mg, 1.459 mmol) in DMF/CH2Cl2 at rt was added EDCI.HCl (363 mg, 1.896 mmol) followed by HOBt.H2O (197 mg, 1.459 mmol). After one minute, (4-fluorophenyl)methanamine (183 mg, 1.459 mmol) was added to the mixture and the reaction mixture was stirred at rt for 4 h. To the reaction mixture were added EtOAc and aq. NaHCO3. The EtOAc layer was separated, washed with water, dried over MgSO4 and concentrated in vacuo to obtain a crude product as a light yellow solid (585 mg, >100% yield), MS: M+H=382.21. The crude product was used directly in the next step without further purification. 1H NMR (CDCl3): δ 8.39 (s, 1H), 8.32 (s, 1H), 7.58˜7.02 (m, 9H), 4.63 (d, J=6.0 Hz, 2H), 3.95 (s, 3H).

1. customThe EtOAc layer was separated
2. washwashed with water
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo