反应详情

温度

40 °C

To a solution of (E)-(6-methoxyindan-1-ylidene)acetonitrile (1.60 g, 8.64 mmol.) in ethanol (80 ml) were added a 2M ammonia/methanol solution (40 ml) and Raney cobalt (1.6 g). The reaction mixture was stirred, under hydrogen atmosphere (4 kgf/cm2) for 32 hours at 40° C. and for further 8 hours at 70° C. The Raney cobalt was filtered off, and then the solvent was distilled off. The residue was purified by means of a silica gel column chromatography (chloroform:methanol=9:1 to chloroform:methanol:triethylamine=90:8:2) to afford the titled compound (1.40 g, yield 86%, oily).

1. waitfor further 8 hours at 70° C
2. filtrationThe Raney cobalt was filtered off
3. distillationthe solvent was distilled off
4. customThe residue was purified by means of a silica gel column chromatography (chloroform:methanol=9:1 to chloroform:methanol:triethylamine=90:8:2)