反应详情

A mixture of 3-chloro-2-nitro-phenylamine (172.6 mg, 1 mmol) and 1-methyl-piperazine (1.5 mL) was heated at 200° C. in a Biotage Initiator Sixty microwave reactor for 15 min, cooled to the room temperature, and concentrated under reduced pressure. The residue was purified by chromatography (500:10:1 CH2Cl2/MeOH/28% aqueous NH4OH) to afford the title compound (139 mg, 59%). 1H NMR (MeOH-d4) δ 2.32 (s, 3H), 2.55 (m, 4H), 2.99 (m, 4H), 6.45 (d, J=9 Hz, 1H), 6.57 (d, J=9 Hz, 1H), 7.15 (dd, J=9 Hz and 9 Hz, 1H). ESI-MS m/z 237.3 (MH+).

1. concentrationconcentrated under reduced pressure
2. customThe residue was purified by chromatography (500:10:1 CH2Cl2/MeOH/28% aqueous NH4OH)