反应详情

To a solution of 1-benzyl-3-oxo-piperidine-4-carboxylic acid ethyl ester hydrochloride (2.11 g, 7.1 mmol) in EtOH (35 mL) was added diethyl guanidinium trifluoroacetate (1.5 g, 7.1 mmol) and sodium ethoxide (21 wt % in EtOH, 6.7 mL). The reaction was heated at reflux for 16 h then cooled to room temperature (rt). The reaction mixture was diluted with H2O and extracted with CH2Cl2 (2×). The combined organic extracts were dried and concentrated. The resulting material was triturated with Et2O to give the title compound (1.54 g, 70%) as a light brown solid. MS (ESI): mass calcd. for C18H24N4O, 312.4; m/z found, 313.3 [M+H]+.

1. temperatureThe reaction was heated
2. temperatureat reflux for 16 h
3. extractionextracted with CH2Cl2 (2×)
4. customThe combined organic extracts were dried
5. concentrationconcentrated
6. customThe resulting material was triturated with Et2O