[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][N:6]([CH2:9][C:10]#[N:11])[CH2:5][CH2:4]1>[Ni].CCO>[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][N:6]([CH2:9][CH2:10][NH2:11])[CH2:5][CH2:4]1A mixture of nitrile 287 (10.25 g, 66.5 mmol) and Raney Nickel (50% w/w in water, ca. 10 mL) in EtOH (150 mL) and cNH3 (10 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 288 as an oil which was used directly.
Wird geladen…