反应详情

To a solution of 100 mg (0.23 mol) of 4-iodo-1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazole in 16 ml of dioxane and 4 ml of water, 90 mg (0.46 mmol) of 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine, 52 mg (0.046 mmol) of palladium tetrakis and 150 mg (0.46 mmol) mg of cesium carbonate were added successively. The mixture was submitted to microwave irradiation at 120° C. for 30 minutes in a sealed vial. The reaction was filtered through a celite pad and the solvent evaporated to dryness. The crude was then partitioned between dichloromethane and water, the organic layer dried over sodium sulphate and the solvent removed in vacuo. After purification by flash-chromatography on a silica gel column (CH2Cl2—CH3COCH3) 78 mg (88%) of the title compound were obtained.

1. customirradiation at 120° C. for 30 minutes in a sealed vial
2. filtrationThe reaction was filtered through a celite pad
3. customthe solvent evaporated to dryness
4. customThe crude was then partitioned between dichloromethane and water
5. dry with materialthe organic layer dried over sodium sulphate
6. customthe solvent removed in vacuo
7. customAfter purification by flash-chromatography on a silica gel column (CH2Cl2—CH3COCH3) 78 mg (88%) of the title compound
8. customwere obtained