反应详情

4-[2-(3-Methylpyridin-4-ylamino)-ethyl]-3-oxo-piperazine-1-carboxlic acid benzyl ester (0.20 g, 0.54 mmol) is dissolved in anhydrous ethanol (20 mL) and hydrogenated at 50 PSI with 10% Pd/C overnight. After filtration, the filtrate is concentrated. The residue is treated with Pd black in 5% HCO2H/CH2Cl2 (10 ml) for 10 minutes. Filtration and concentration gives crude residue, which is purified by chromatography using NH4OH/MeOH/CH2Cl2 (1:5:95) to give the title compound as a clear syrup (0.078 g, 0.33 mmol). 1H NMR (CDCl3, 300 MHz) δ8.17 (d, 1H), 8.03 (s, 1H), 7.35 (s, 5H), 6.36 (d, 1H), 5.30 (b, 1H), 3.74 (t, 2H), 3.53 (s, 2H), 3.38 (m, 4H), 3.08 (t, 2H), 2.02 (s, 3H).

1. filtrationAfter filtration
2. concentrationthe filtrate is concentrated
3. additionThe residue is treated with Pd black in 5% HCO2H/CH2Cl2 (10 ml) for 10 minutes
4. filtrationFiltration and concentration
5. customgives crude residue, which
6. customis purified by chromatography