反应详情

A mixture of nitrile 290 (5.58 g, 40.4 mmol) and Raney Nickel (50% w/w in water, ca. 5 mL) in EtOH (50 mL) and cNH3 (4 mL) was stirred under H2 (60 psi) for 16 h. The mixture was filtered through Celite, washed with EtOH (3×10 mL) and the solvent evaporated to give crude diamine 291 as an oil (2.03 g, 35%) which was used without further purification: 1H NMR δ 2.72 (t, J=6.1 Hz, 2H, CH2N), 2.60-2.68 (m, 4H, 2×CH2N), 2.53 (t, J=6.1 Hz, 2H, CH2N), 1.55-1.66 (m, 10H, 4×CH2, NH2).

1. filtrationThe mixture was filtered through Celite
2. washwashed with EtOH (3×10 mL)
3. customthe solvent evaporated