反应详情

温度

40 °C

[2-(4-Methyl-piperazin-1-yl)-5-nitro-pyridin-4-yl]-acetic acid ethyl ester (250 mg, 0.81 mmol) is dissolved in methanol (2.5 ml). An aqueous solution of ammonia (25%, 2.5 ml) is added, and the mixture is warmed to 40° C. for 18 h. TLC analysis indicated complete conversion of the starting material. Solvents are removed, and the residue is purified by FCC (CH2Cl2/MeOH, gradient from 97:3 to 90:10) to afford the title compound. 1H NMR (d6-DMSO, 400 MHz): δ 2.21 (s, 3H), 2.38 (m, 4H), 3.72 (m, 4H), 3.80 (s, 2H), 6.84 (s, 1H), 6.93 (s, broad, 1H), 7.46 (s, broad, 1H), 8.85 (s, 1H). ES+−MS: 280.3 [M+H]+, ES−−MS: 278.3 [M−H]−.

1. customSolvents are removed
2. customthe residue is purified by FCC (CH2Cl2/MeOH, gradient from 97:3 to 90:10)