反应详情

To a solution of 4-amino-N-ethyl-5-nitronicotinamide (CXXVII) (180 mg, 0.856 mmol) in MeOH (5 mL) was added 10% Pd/C (27 mg, 15% by wt). The solution was purged with hydrogen and stirred for 16 h at room temperature under hydrogen. The suspension was filtered through Celite and concentrated under vacuum. The residue was purified on a silica gel column (100% CHCl3→10:90 MeOH[7N NH3]:CHCl3) to produce 4,5-diamino-N-ethylnicotinamide (CXXVIII) as a dark yellow solid (80 mg, 0.44 mmol, 51.9% yield). 1H NMR (DMSO-d6, 500 MHz) δ ppm 1.14 (t, J=7 Hz, 3H), 3.92 (q, J=7 Hz, 2H) 5.56 (brs, 2H), 6.60 (brs, 1H), 7.66 (s, 1H), 8.30 (s, 1H); ESIMS found C8H12N4O m/z 181 (M+H).

1. customThe solution was purged with hydrogen
2. filtrationThe suspension was filtered through Celite
3. concentrationconcentrated under vacuum
4. customThe residue was purified on a silica gel column (100% CHCl3→10:90 MeOH[7N NH3]:CHCl3)