反应详情

温度

50 °C

tert-Butyl 2-nitro-4-((tetrahydrofuran-2-yl)methylcarbamoyl)benzyl(2-(pyridin-2-yl)ethyl)carbamate, from above, (238 mg, 0.492 mmol) and SnCl2.2H2O (279 mg, 1.23 mmol) were suspended in ethanol (1.6 mL) and stirred at 50° C. for 1 hour. The reaction mixture was concentrated to dryness, re-suspended in ethyl acetate, washed with water and brine, dried over anhydrous Na2SO4, concentrated onto silica gel and purified by flash chromatography (20 methanol:1 triethylamine:79 dichloromethane isocratic) to afford the desired intermediate, tert-butyl 2-amino-4-((tetrahydrofuran-2-yl)methylcarbamoyl)benzyl(2-(pyridin-2-yl)ethyl)carbamate (103 mg). LC/MS: Calc. C25H34N4O4 454.25 amu; Obs. [M+H]+=455.5 amu.

1. concentrationThe reaction mixture was concentrated to dryness
2. washwashed with water and brine
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated onto silica gel
5. custompurified by flash chromatography (20 methanol:1 triethylamine:79 dichloromethane isocratic)