反应详情

温度

70 °C

To a solution of 3-oxo-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid ethyl ester (3.0 g, 15.23 mmol) in methanol (20 mL) was added 5 mL Raney Nickel (50% aq slurry). The resultant mixture was degassed and charged with hydrogen (g) three times, heated to 70° C. and stirred for 12 hrs. The suspension was filtered through celite, and concentrated to provide a white solid (3.0 g, 100%). 1H NMR (300 MHz, CDCl3) δ ppm 1.25 (t, J=7.0 Hz, 3H), 1.57 (m, 2H), 1.72 (app dd, J=1.4, 15.1 Hz, 2H), 1.94 (m, 2H), 2.12 (m 4H), 4.13 (q, J=7.1 Hz, 2H), 4.25 (m, 2H); MS (ESI+Q1MS) m/z 200 [M+H]+

1. customThe resultant mixture was degassed
2. additioncharged with hydrogen (g) three times
3. filtrationThe suspension was filtered through celite
4. concentrationconcentrated