反应详情

To a solution of [4-(4-methoxy-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester (11.7 g, 38 mmol, 1 eq.) in 154 mL of EtOH was added a solution of NaOH (3.07 g, 77 mmol, 2 eq.) in 154 mL of H2O. The resulting mixture was stirred at room temperature overnight. After 18 h, the reaction mixture was concentrated and treated with 1 N HCl to pH 5. The resulting mixture was freeze dried using lyophilizer to remove H2O. The resulting yellow solids were washed with dichloromethane/methanol and filtered off NaCl. The filtrate was concentrated to give the title compound as a white solid (11 g, 38 mmol). Exact mass calculated for C15H20N1O4 278.1. MS (ESI) m/z 278.8 (M+H)+.

1. waitAfter 18 h
2. concentrationthe reaction mixture was concentrated
3. additiontreated with 1 N HCl to pH 5
4. customdried
5. customto remove H2O
6. washThe resulting yellow solids were washed with dichloromethane/methanol
7. filtrationfiltered off NaCl
8. concentrationThe filtrate was concentrated