反应详情

温度

135 °C

2-[3-Bromo-2-(tert-butyl-dimethyl-silanyloxymethyl)-phenyl]-7-(1-methyl-cyclopropyl)-2H-isoquinolin-1-one (0.102 g, 0.205 mmol) and 1-Methyl-3-[5-(morpholine-4-carbonyl)-pyridin-2-ylamino]-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-1H-pyridin-2-one (0.1 g, 0.227 mmol) were dissolved in 2.5 ml dioxane under heating; 0.5 ml of water followed by cesium carbonate (0.259 g, 0.795 mmol) were added. After that [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex (0.019 g, 0.023 mmol) was added and heated to 135° C. for 30 min by microwave. The reaction mixture was filtered over cellulose; washed with dioxane; concentrated; residue was purified by 24 g silica gel chromatography (gradient elution dichloromethane for 5 min, then 0-10% methanol in dichloromethane during in 25 min, then dichloromethane 9:1 methanol for 10 min) to yield 2-(2-tert-Butyl-dimethyl-silanyloxymethyl)-3-{1-methyl-5-[5-(morpholine-4-carbonyl)-pyridin-2-ylamino]-6-oxo-1,6-dihydro-pyridin-3-yl}-phenyl)-6-(1-methyl-cyclopropyl)-2H-isoquinolin-1-one (0.095 g, 0.13 mmol) MS (ESI) 732.2 (M+H)+

1. temperatureunder heating
2. additionwere added
3. additionAfter that [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex (0.019 g, 0.023 mmol) was added
4. filtrationThe reaction mixture was filtered over cellulose
5. washwashed with dioxane
6. concentrationconcentrated
7. customresidue was purified by 24 g silica gel chromatography (
8. washgradient elution dichloromethane for 5 min