反应详情

2.3 g (0.0113 mol) 1-(2-Aminophenyl)-2-cyclopropylcyclobutanol (prepared as described in Example 4) was dissolved in 40 ml of ethanol, 3.25 g sulphuric acid (96%) was added and after the addition of 500 mg of 10% Pd on charcoal, the mixture was hydrogenated for 1 hour at room temperature. After removal of the catalyst, ethanol was distilled off in a water jet vacuum and the residue purified by flash chromatography over silica gel (eluant: hexane/ethyl acetate 4:1). Yield: 1.88 g (89% of theory) of the cis isomer of 2-(2-cyclopropylcyclobutyl)phenylamine in form of a yellow oil (1HNMR (CDCl3): −0.1-0.05 ppm/m/2H, 0.19 ppm/m/1H, 0.27 ppm/m/1H, 0.55 ppm/m/1H, 1.65 ppm/m/1H, 2.15 ppm/m/3H, 2.52 ppm/m/1H, 3.55 ppm (broad)/2H −NH2, 6.68 ppm/d/1H, 6.80 ppm/t/1H, 7.08 ppm/t/1H, 7.18 ppm/d/1H).

1. customAfter removal of the catalyst, ethanol
2. distillationwas distilled off in a water jet vacuum
3. customthe residue purified by flash chromatography over silica gel (eluant: hexane/ethyl acetate 4:1)