反应详情

温度

70 °C

2,4-Dichloro-7-iodo-quinoline (1.7 g, 5.26 mmol) and 4-(3-mercapto-phenyl)-tetrahydro-pyran-4-carbonitrile (1p, 1.27 g, 5.79 mmol) were dissolved in 1,4-dioxane (50 mL) and degassed with N2 for 10 minutes. Pd2dba3 (120 mg, 0.13 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (150 mg, 0.27 mmol) were added, followed by iPr2NEt (1.4 mL, 7.9 mmol), and the reaction was heated to 70° C. for 2 hours. The mixture was diluted with EtOAc and water, and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the residue was purified by silica gel chromatography to give the desired product, 1q.

1. customdegassed with N2 for 10 minutes
2. extractionthe aqueous layer was extracted with EtOAc
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customthe residue was purified by silica gel chromatography