反应详情

Ethyl 4-(6-oxo-piperidin-3-yl)-benzoate (320 mg, 1.30 mmol, reference example 66) is dissolved in MeOH (8 mL). To this solution is added 1 N NaOH (1.43 mL, 1.43 mmol) and the resulting solution stirred at room temperature for 1 hour. An additional portion of 1 N NaOH (2 mL) is added and the mixture allowed to stir at room temperature overnight (16 hours). 1 N HCl is added until pH 2-3 is reached. A precipitate formed and is filtered, washed with water and placed in a vacuum oven to dry overnight to afford the title compound (250 mg, 88%) as small white crystals (needles). 1H NMR (300 MHz, DMSO) δ 1.94 (m, 2H), 2.23 (m, 2H), 3.06 (m, 1H), 3.23 (m, 2H), 7.42 (d, J=8.3, 2H), 7.57 (bs, 1H), 7.87 (d, J=8.1, 2H); MS (Ion spray) m/z 220 (M+H)+.

1. stirringto stir at room temperature overnight (16 hours)
2. customA precipitate formed
3. filtrationis filtered
4. washwashed with water
5. customto dry overnight