反应 #3402611
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08716287B2
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Ethanolamine (0.86 g, 14.07 mmol) was added to a solution of 2,4-difluorobenzaldehyde (2.0 g, 14.07 mmol) in methanol (50 mL) at RT. Sodium bicarbonate (7.0 g, 83.33 mmol) was added and the reaction mixture was stirred at reflux for 24 hours. The mixture was cooled to 0° C. and sodium borohydride (0.32 g, 8.42 mmol) was then added in lots, maintaining the temperature of the mixture at 0-5° C. The reaction mixture was allowed to warm to RT over a period of 4 hours. The reaction mixture was then diluted with DCM (50 mL), washed with brine (2×30 mL), dried (Na2SO4) and the solvents removed under reduced pressure to afford the title compound (1.79 g, 69%). The product was used in the next step without further purification. at reflux for 24 hours maintaining the temperature of the mixture at 0-5° C to warm to RT over a period of 4 hours washed with brine (2×30 mL) dried (Na2SO4) the solvents removed under reduced pressure
来源 ID: ord-f1c9c72b40d843b3ba71edba9d6e18e9