反应详情

To compound 1 (50 mg, 0.079 mmol) in DMF (2 mL) was added 2 (49 mg, 0.085 mmol) and HATU (33 mg, 0.086 mmol) followed by adding DIPEA (45 uL) and the reaction mixture was stirred for 4 hrs at room temperature. 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 (47 mg, 60%). MS: (M+H)+ 1003.

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