反应详情

温度

120 °C

To a degassed solution of 9-methyl-2,3,4,5,6,10c-hexahydro-1H-3a,6-diaza-cyclopenta[c]fluorene (50 mg, 0.22 mmol), potassium phosphate (100 mg, 0.462 mmol), L-proline (5 mg, 0.022 mmol) and copper iodide (5 mg, 0.044 mmol) in DMF (1 mL) was added 5-(2-bromo-1-methyl-vinyl)-2-methyl-pyridine (80 mg, 0.375 mmol). The reaction mixture was stirred at 120° C. for 20 h. The progress of reaction was monitored by TLC and LCMS. The reaction mixture was diluted with water (20 mL) and extracted with EtOAc (3×10 mL). The organic layer was washed with water (3×10 mL), followed by brine (15 mL), dried over anhydrous Na2SO4 and evaporated under reduced pressure. The residue was purified by reverse phase HPLC;

1. customThe progress of reaction
2. extractionextracted with EtOAc (3×10 mL)
3. washThe organic layer was washed with water (3×10 mL)
4. dry with materialdried over anhydrous Na2SO4
5. customevaporated under reduced pressure
6. customThe residue was purified by reverse phase HPLC