反应详情

A mixture of (5)-1-(4′-trifluoromethyl-biphenyl-3-yl)ethylamine hydrochloride (75 mg, 0.25 mmol), (S)-1-(4-fluoro-benzenesulfonyl)-pyrrolidine-2-carboxylic acid (68 mg, 0.25 mmol), N-(3-dimethylamniopropyl)-N′-ethylcarbodiimide hydrochloride (71 mg, 0.37 mmol), 1-hydroxybenzotriazole (50 mg, 0.37 mmol) and DMF (2 mL) was added Et3N (0.10 mL, 0.75 mmol). After 12 h, MeOH (0.5 mL) was added to the reaction mixture and resulting solution was purified by preparative reverse-phase HPLC to afford (70 mg, 54%) of a white solid. MS (ESI): mass calcd. for C26H24F4N2O3S, 520.1; m/z found, 521.1 [M+H]+. 1H NMR (500 MHz, CDCl3) δ 7.93-7.87 (m, 2H), 7.79 (d, J=8.0, 2H), 7.73-7.66 (m, 3H), 7.54 (d, J=7.6, 1H), 7.49 (t, J=7.6, 1H), 7.44 (d, J=7.6, 1H), 7.35 (d, J=8.0, 1H), 7.30-7.23 (m, J=8.7, 1H), 5.27-5.11 (m, 1H), 4.11 (dd, J=8.9, 3.1, 1H), 3.71-3.60 (m, 1H), 3.26-3.15 (m, 1H), 2.28-2.17 (m, 1H), 1.91-1.75 (m, 1H), 1.74-1.64 (m, 2H), 1.60 (d, J=7.0, 3H).

1. customresulting solution
2. customwas purified by preparative reverse-phase HPLC