反应详情

温度

50 °C

A mixture of 4-(6-bromo-1-oxo-4-phenyl-3-propionyl-1H-isoquinolin-2-ylmethyl)benzenesulfonamide (0.10 g), potassium carbonate (0.11 mg), 1-piperidinecarbonyl chloride (29 μl) and DMF (2.0 ml) was stirred at 50° C. for 18 hrs. After the completion of the reaction, the reaction mixture was concentrated, and the residue was diluted with dichloromethane. Then, this solution was washed with 1N hydrochloric acid, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by medium pressure preparative LC (hexane/ethyl acetate=4/1-1/1) to give the title compound (38 mg) as a colorless powder. HPLC analysis: purity 91.6% (retention time: 4.78 min). MS (ESI+): 636 (M+H), 638.

1. customAfter the completion of the reaction
2. concentrationthe reaction mixture was concentrated
3. additionthe residue was diluted with dichloromethane
4. washThen, this solution was washed with 1N hydrochloric acid
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by medium pressure preparative LC (hexane/ethyl acetate=4/1-1/1)