反应 #3031429
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05922697
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To N-(t-Butyloxycarbonyl)-2-(2-methoxyphenyl)-ethylamine (182.7 mmol, 45.9 g) in dry tetrahydrofuran (200 mL) at 0° C. was added, in portions, lithium aluminum hydride (219.2 mmol, 8.3 g) under N2. After stirring at 0° C. for 1 hour, the ice-bath was removed and then the reaction heated to reflux for 24 hours, cooled to room temperature then to 0° C.; the excess lithium aluminum hydride was destroyed very carefully with 20% potassium hydroxide solution (1.3 equivalent). After removing the salt by filtration, the filtrate was dried then evaporated to dryness to give product as a white solid (26.2 g, 87%). the ice-bath was removed the reaction heated to reflux for 24 hours cooled to room temperature to 0° C. After removing the salt by filtration the filtrate was dried then evaporated to dryness
来源 ID: ord-7bdd198fd2c54cdbbacc8d539aa6f59a