反应详情

Diphosphoryl chloride (23.5 mL, 170 mmol) was added dropwise to a stirred mixture of 4-nitroindole (25.0 g, 154 mmol) and ethyl 1-piperidineglyoxylate (29.0 g, 170 mmol) at 0° C. The mixture was allowed to warm slowly to ambient temperature and stirring was continued for 18 h. The reaction mixture was cooled to 0° C. and quenched carefully by addition of EtOH (50 mL), followed by saturated aqueous NaHCO3 until no further effervescence was observed. The precipitated yellow solid was isolated by filtration, washed with H2O, and dried in vacuo to give the title compound. MS: m/z=263 (M+1).

1. temperatureThe reaction mixture was cooled to 0° C.
2. customquenched carefully by addition of EtOH (50 mL)
3. customThe precipitated yellow solid was isolated by filtration
4. washwashed with H2O
5. customdried in vacuo