反应详情

温度

70 °C

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+)

1. concentrationSolvents concentrated
2. customwhite powder that resulted
3. customThe white solid that resulted from the reduction
4. customReaction
5. customReaction
6. temperaturecooled to 0° C.
7. extractionProduct extracted out with CHCl3, and extracts
8. dry with materialdried with Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo