反应详情

温度

25 °C

A solution of 1 (47 mg, 0.06 mmol), 2 (40 mg, 0.078 mmol) and BOP (34.5 mg, 0.078 mmol) in DMF (3 ml) was treated with DIPEA (68 uL). The reaction mixture was stirred at 25° C. for 30 min. The solvent was removed and was further dried in high vacuo for 4 h. The solvent was removed under vacuo and the crude product was purified by Prep HPLC (SymmetrPrep C18, 7 μm, 19×150 mm column), eluted at 10 ml/min (0.01% TFA in water/acetonitrile) with a gradient: 10% acetonitrile in 5 min, 10% to 50% acetonitrile in 15 min, maintaining 50% acetonitrile in 5 min, 50% to 100% acetonitrile in 5 min, to give 3 (56 mg, 85%). MS: calcd for C56H54BrN9O8 (M+H) m/z 1060.33 found 1060.44.

1. customThe solvent was removed
2. customwas further dried in high vacuo for 4 h
3. customThe solvent was removed under vacuo
4. customthe crude product was purified by Prep HPLC (SymmetrPrep C18, 7 μm, 19×150 mm column)
5. washeluted at 10 ml/min (0.01% TFA in water/acetonitrile) with a gradient
6. wait10% acetonitrile in 5 min
7. wait10% to 50% acetonitrile in 15 min
8. temperaturemaintaining 50% acetonitrile in 5 min
9. wait50% to 100% acetonitrile in 5 min