反应详情

温度

25 °C

To compound 1 (18.2 mg, 0.03 mmol) in DMF (2 mL) was added 2 (16 mg, 0.036 mmol) and HATU (14 mg, 0.036 mmol) followed by adding DIPEA (19 uL) and the reaction mixture was stirred for 7 hrs at 25° C. The solvent was removed under vacuo and the 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 (15.8 mg, 53%). MS: calcd for C59H58ClN7O9 (M+H) m/z 1044.4 found 1045.

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