反应详情

温度

0 °C

Benzyl chloroformate (0.06 ml, 0.420 mmol) was added to a flask containing tert-butyl(2-{[4-(aminomethyl)benzoyl]amino}-6-phenylpyridin-3-yl)carbamate (158 mg, 0.378 mmol) and DIPEA (0.15 ml, 0.859 mmol) in THF (5 mL) at 0° C. The mixture was stirred at 0° C. for 1 hour. Water was added and the products were extracted into EtOAc (2×). The combined organic extracts were washed with brine, dried over sodium sulfate and concentrated. The organic product was purified by column chromatography on silica gel Biotage 25S, eluting with EtOAc/hexanes (0%-100%) to give a pale slightly yellow transparent gel. MS: cal'd 553 (MH+), exp 553 (MH+).

1. extractionthe products were extracted into EtOAc (2×)
2. washThe combined organic extracts were washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. customThe organic product was purified by column chromatography on silica gel Biotage 25S
6. washeluting with EtOAc/hexanes (0%-100%)
7. customto give a pale slightly yellow transparent gel