反应详情

1,2-Phenylenediacetonitrile (7.5 g, 48 mmol) dissolved in ethanol (150 ml) was added to Raney Ni (2 g) which had been previously washed with ethanol (3×20 ml). The mixture was then hydrogenated at 50° C. at 50 psi pressure with shaking for 24 h. The reaction mixture was then cooled to room temperature and filtered through a pad of kieselguhr and washed through with ethanol (100 ml). The filtrate was evaporated in vacuo to give a brown oil which was chromatographed on silica gel (100 g), eluting with 2-10% methanol in CH2Cl2 to give the title compound as a brown oil (2.45 g, 35%).

1. washhad been previously washed with ethanol (3×20 ml)
2. customwas then hydrogenated at 50° C. at 50 psi pressure
3. filtrationfiltered through a pad of kieselguhr
4. washwashed through with ethanol (100 ml)
5. customThe filtrate was evaporated in vacuo
6. customto give a brown oil which
7. customwas chromatographed on silica gel (100 g)
8. washeluting with 2-10% methanol in CH2Cl2