反应详情

温度

25 °C

A solution of 3 (22 mg, 0.02 mmol) in DMF (2 mL) was treated with 5% piperidine in DMF (2 mL). The reaction mixture was stirred for 5 min at 25° C. The final 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 obtain 4 (16.2 mg, 93%). MS: calcd for C41H44BrN9O6 (M+H) m/z 838.26 found 839.2.

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