反应详情

温度

120 °C

tert-Butyl (1-(4-(8-chloro-4-oxo-2-phenyl-4H-pyrano[2,3-c]pyridin-3-yl)phenyl)cyclobutyl)carbamate (63 mg, 0.115 mmol), imidazole (11 mg, 0.161 mmol), cesium carbonate (75 mg, 0.23 mmol) and copper (II) iodide (5 mg, 0.023 mmol) were dissolved in DMF (1 mL) in a microwave vial. The vial was sealed, evacuated and flushed twice with nitrogen. The reaction mixture was heated conventionally at 120° C. for 72 h. After cooling to RT, the resultant mixture was diluted with EtOAc, washed with water, dried (Na2SO4), filtered and concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, 1:1 ethyl acetate/hexane) to give the title compound (20 mg, 24%). LCMS (Method I): RT=5.89 min, [M+H]+=535.

1. customThe vial was sealed
2. customevacuated
3. customflushed twice with nitrogen
4. temperatureAfter cooling to RT
5. additionthe resultant mixture was diluted with EtOAc
6. washwashed with water
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo