反应详情

温度

90 °C

To a solution of 3-aminophthalic acid (0.100 g, 0.552 mmol) in DMF (1.1 mL) was added 3-aminopiperidine-2-one (0.063 g, 0.552 mmol) and the reaction was stirred at 90° C. over 18 h. Volatiles were removed in vacuo and the dark-brown crude residue was purified by preparative reverse phase HPLC to give the desired product 28 (0.050 g, 35%) as an off-white powder. 1H NMR (400 MHz, DMSO) δ 7.83 (s, 1H), 7.43 (dd, J=8.3, 7.1 Hz, 1H), 7.07-6.87 (m, 2H), 6.47 (br s, 2H), 4.49 (dd, J=11.9, 6.3 Hz, 1H), 3.27-3.10 (m, 2H), 2.19 (dt, J=12.0, 7.7 Hz, 1H), 2.05-1.72 (m, 3H). MS (ESI) m/z calcd for C13H14N3O3 [M+H]+ 260.3, found: 260.9.

1. customVolatiles were removed in vacuo
2. customthe dark-brown crude residue was purified by preparative reverse phase HPLC