反应详情

温度

90 °C

In a flask was placed tert-butyl 5-bromonicotinate (1.00 g, 3.87 mmol), 10% w/w palladium on carbon (210 mg, ˜0.2 mmol Pd), potassium carbonate (1.10 g, 7.96 mmol), 3,4-methylenedioxy-phenyl boronic acid (0.96 g, 5.79 mmol), dimethylformamide (50 mL) and water (250 L). The flask was purged with nitrogen and then heated, with stirring, to 90° C. for 15 hr. The reaction mixture was allowed to cool, diluted with water (350 mL) and extracted with CH2Cl2 (4X). The combined extracts was washed with water, dried (MgSO4) and concentrated in vacuo. The crude residue was purified by flash chromatography on silica (gradient, CH2Cl2 to 50% ether/CH2Cl2) to provide an off-white solid (1.02 g, 88%).

1. customIn a flask was placed
2. customThe flask was purged with nitrogen
3. temperatureheated
4. temperatureto cool
5. additiondiluted with water (350 mL)
6. extractionextracted with CH2Cl2 (4X)
7. washThe combined extracts was washed with water
8. dry with materialdried (MgSO4)
9. concentrationconcentrated in vacuo
10. customThe crude residue was purified by flash chromatography on silica (gradient, CH2Cl2 to 50% ether/CH2Cl2)