反应详情

6-(4,5-Methylenedioxy-2-nitrophenyl)-2,3-dimethoxynaphthalene (25 mg, 0.071 mmol) was hydrogenated overnight in ethyl acetate (40 mL) at 40˜45 lb./sq. in. under catalysis of palladium (10 wt % on activated carbon, 20 mg). The solution was passed through celite bed and the catalyst was washed with ethyl acetate (3×10 ml). Concentration in vacuo gave the crude product. Chromatography using 60:40 hexanes:ethyl acetate gave compound 13 (15 mg) in 66% yield; 1H NMR (CDCl3) d 4.01(3H, s), 4.02(3H, s), 5.91(2H, s), 6.40(1H, s), 6.73(1H, s), 7.13(1H, s), 7.15(1H, s), 7.39(1H, dd, J=8.2, J=1.8), 7.72(1H, s), 7.74(1H, d, J=8.5); 13C NMR d 56.4, 98.3, 101.2, 106.6, 106.8, 110.7, 120.5, 126.3, 127.0, 127.3, 128.5, 129.9, 135.7, 138.9, 141.1, 148.0, 150.1, 150.3.

1. washthe catalyst was washed with ethyl acetate (3×10 ml)
2. concentrationConcentration in vacuo
3. customgave the crude product