反应详情

A round bottom flask was charged with (R)-2-(5-amino-1-oxoisoquinolin-2(1H)-yl)-2-phenylacetamide (120 mg, 0.00041 mol), N,N-dimethylformamide (1.5 mL, 0.019 mol), N,N-diisopropylethylamine (0.1 mL, 0.0008 mol), N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (0.3 g, 0.0008 mol) and (S)-2-(3,4-dichlorophenyl)propanoic acid (0.11 g, 0.00049 mol) and the reaction stirred at room temperature overnight. The solvent was removed and the residue purified by flash chromatography and again by preparative HPLC (reverse phase) to obtain the product as a white solid. MS m/z=495.2 (M+H). 1H NMR (400 MHz; DMSO-d6) δ 9.98 (s, 1H), 8.13-8.11 (d, J=8.37 Hz, 1H), 8.03 (s, 1H), 7.74-7.72 (d, J=7.90 Hz, 1H), 7.64-7.63 (d, J=2.06 Hz, 1H), 7.61-7.59 (d, J=7.94 Hz, 1H), 7.55 (s, 1H), 7.50-7.33 (m, 6H), 7.00-6.98 (d, J=8.02 Hz, 1H), 6.74 (s, 1H), 6.39-6.37 (d, J=8.02 Hz, 1H), 4.02-3.96 (q, J=7.01 Hz, 1H), 1.45-1.43 (d, J=7.55 Hz, 3H).

1. customThe solvent was removed
2. customthe residue purified by flash chromatography and again by preparative HPLC (reverse phase)