反应 #3721498
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06310095B1
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of Boc-homophenylalanine (3.00 g, 10.8 mmol) in CH2Cl2 at room temperature was added a solution of 4N HCl in dioxane (20 mL, 80 mmol), and mixture stirred overnight. Solvents concentrated, and white powder that resulted was reduced under high pressure (4 atm. H2) using platinum/HCl. The white solid that resulted from the reduction was mixed with aqueous 4N NaOH (30 mL), water (30 mL), and THF (50 mL) at room temperature, and to this was added di-t-butyl dicarbonate (3.5 g, 16 mmol). Reaction heated at 70° C. overnight. Reaction cooled to 0° C., and an aqueous solution of 3N HCl added until the pH reached 6. Product extracted out with CHCl3, and extracts dried with Na2SO4, filtered, and concentrated in vacuo to produce a white solid (3.24 g, 106%). m/e (DCI) 286 (MH+) Solvents concentrated white powder that resulted The white solid that resulted from the reduction Reaction Reaction cooled to 0° C. Product extracted out with CHCl3, and extracts dried with Na2SO4 filtered concentrated in vacuo
来源 ID: ord-9c42513025ff49dba74ab9f6c43a8dd9