反应详情

温度

70 °C

To a suspension of (E)-ethyl 3-(2-oxo-2,4-dihydro-1H-spiro[[1,8]naphthyridine-3,4′-piperidine]-6-yl)acrylate (99.8 mg, 0.316 mmol) in 1,2-dichloroethane (5 mL) were added sodium triacetoxyborohydride (139 mg, 0.656 mmol) and paraformaldehyde (21 mg, 0.699 mmol). The reaction mixture was heated to 70° C. for 5 h. After cooling to room temperature, the reaction mixture was partitioned between DCM (25 mL) and water (25 mL). The aqueous layer was separated and extracted with DCM (2×20 mL). The combined organic phases were washed with saturated NaHCO3 (3×25 mL) and brine (25 mL), dried over sodium sulfate and concentrated. The crude product was used directly in the next step.

1. temperatureAfter cooling to room temperature
2. customthe reaction mixture was partitioned between DCM (25 mL) and water (25 mL)
3. customThe aqueous layer was separated
4. extractionextracted with DCM (2×20 mL)
5. washThe combined organic phases were washed with saturated NaHCO3 (3×25 mL) and brine (25 mL)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated