反应详情

温度

80 °C

Into a 3000-mL 4-necked round-bottom flask was placed potassium carbonate (93.2 g, 662 mmol, 0.50 equiv) and DMSO (2000 mL). The resulting solution was heated to 80° C. This was followed by the addition of tert-butyl 4-(2-ethoxy-2-oxoethylidene)piperidine-1-carboxylate (368 g, 1.30 mol, 1.00 equiv, 95%) and CH3NO2 (417 g, 6.70 mol, 5.00 equiv, 98%) slowly. The resulting solution was stirred for 120 min at 90° C. After being cooled to room temperature, the reaction mixture was adjusted to ph 5 with HCl (0.5 mol/L) and diluted with 2000 mL of water. The resulting solution was extracted with 3×1500 mL of ether. The organic layers were combined, washed with 1×2000 mL of water and 1×2000 mL of saturated brine, dried and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with ethyl acetate/petroleum ether (1:20-1:15-1:10) to afford the title compound.

1. customInto a 3000-mL 4-necked round-bottom flask was placed
2. temperatureAfter being cooled to room temperature
3. extractionThe resulting solution was extracted with 3×1500 mL of ether
4. washwashed with 1×2000 mL of water and 1×2000 mL of saturated brine
5. customdried
6. concentrationconcentrated under vacuum
7. washeluted with ethyl acetate/petroleum ether (1:20-1:15-1:10)