反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A 5N aqueous solution of sodium hydroxide (336 mL, 1.68 mol) was added into a solution of 4-(2-methylpiperidin-1-yl)-3-(trifluoromethyl)benzonitrile (28.0 g, 104.4 mmol) in MeOH (280 mL) and the resulting mixture was heated at reflux for 7 hours. The reaction mixture was cooled to 0° C. and acidified to pH 2 with a 5N aqueous solution of HCl. The precipitate was filtered, washed with water and dried under vacuum to give the title compound as a white powder (27.5 g, 91%). HPLC (Method A), Rt 5.4 min (purity: 99.8%). UPLC/MS, M+(ESI): 288.2, M−(ESI): 286.2. 1H NMR (DMSO-d6, 300 MHz) δ 13.30 (bs, 1H), 8.17 (m, 2H), 7.68 (d, J=8.2 Hz, 1H), 3.08 (m, 1H), 3.08 (m, 1H), 2.88 (m, 1H), 2.57 (m, 1H), 1.77-1.25 (m, 6H), 0.72 (d, J=6.0 Hz, 3H).
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureat reflux for 7 hours
- filtrationThe precipitate was filtered
- washwashed with water
- customdried under vacuum