反应详情

温度

80 °C

To a solution of phenyl carbamate (20.0 g, 146 mmol) in MeCN (200 mL) was added N-methylpiperazine (20.00 g, 200 mmol) followed by catalytic amount of ytterbium triflate (0.500 g, 1.061 mmol) and the resulting mixture was heated at 80° C. for 1 h. The solvent from the reaction mixture was completely evaporated and the residue was crystallized from MTBE to provide 4-methylpiperazine-1-carboxamide (14.2 g, 68% yield) as white solid 1H NMR (400 MHz, DMSO-d6): δ 5.92 (s, 2H), 3.42 (t, J=4.9 Hz, 4H), 2.19 (t, J=4.9 Hz, 4H), 2.14 (s, 3H).

1. customThe solvent from the reaction mixture was completely evaporated
2. customthe residue was crystallized from MTBE