反应详情

2-(trimethylsilyl)ethyl 5-[(tert-butoxycarbonyl)amino]pentanoate (317 mg, 1.0 mmol) was treated with 4N HCl in dioxane at room temperature for 30 minutes, then concentrated under reduced pressure. The residue (665 mg, 1.0 mmol), N-acetyl-4-{2-[(benzhydryloxy)carbonyl][tert-butoxy(oxo)acetyl]anilino}-3-ethylphenylalanine (665 mg, 1.0 mmol), 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (321 mg, 1.0 mmol) and diisopropylethylamine (521 μL, 3.0 mmol) in N,N-dimethylformamide (2 mL) was stirred at ambient temperature overnight, diluted with ethyl acetate and washed with aqueous NaHCO3 (1×30 mL), brine (1×30 mL), dried (MgSO4), filtered and concentrate under reduced pressure. The residue was purified on silica gel eluting with ethyl acetate to provide of titled compound 480 mg. MS (APCI(+)) m/e 864 (M+H)+.

1. concentrationconcentrated under reduced pressure
2. washwashed with aqueous NaHCO3 (1×30 mL), brine (1×30 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrate under reduced pressure
6. customThe residue was purified on silica gel eluting with ethyl acetate