反应详情

To a microwave vial containing 5-bromo-N-(3(dimethylamino)propyl) isoquinolin-1-amine (Step 5, 0.055 g, 0.2 mmol) in 1,4-Dioxane (2 mL), was added N-(6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)naphthalen-2-yl)thiophene-3-carboxamide (0.100 g, 0.3 mmol), Fibrecat catalyst (0.005 g, 5% by wt.), along with 2 M Potassium Carbonate (0.5 mL, 1 mmol). The reaction mixture was placed into CEM Microwave for 10 minutes at 80° C., while supplying 60 Watts of energy via power-max. The mixture was diluted with DCM and H2O, and extracted with DCM (3×10 mL). Then dried organics (over sodium sulfate), was filtered, and concentrated in-vacuo. The crude was purified on reverse-phase HPLC. This gave an off-white amorphous solid after drying, which was titled product (0.023 g, 0.08 mmol). MS (ESI pos. ion) m/z: 481 (M+H). Calc'd Exact Mass for C29H28N4OS: 480

1. extractionextracted with DCM (3×10 mL)
2. filtrationThen dried organics (over sodium sulfate), was filtered
3. concentrationconcentrated in-vacuo
4. customThe crude was purified on reverse-phase HPLC
5. customThis gave an off-white amorphous solid
6. customafter drying