反应详情

温度

90 °C

A stirred mixture of 2,5-dibromopyridin-3-amine (860 mg, 3.41 mmol), 4-methoxyphenylboronic acid (519 mg, 3.41 mmol), trans-dichlorobis(triphenylphosphine)palladium (II) (120.5 mg, 0.17 mmol), and 2.0M sodium carbonate (5.1 mL, 10.2 mmol) in 1,4-dioxane (15 mL) was heated to 90° C. After 19 h, the reaction was cooled to rt then diluted with water. After extraction with EtOAc, the organic extraction was dried over anhydrous sodium sulfate. After filtration and concentration, the residue was purified on silica gel (0-20% EtOAc in hexanes) to afford a white solid as 5-bromo-2-(4-methoxyphenyl)pyridin-3-amine. 1H NMR (400 MHz, CDCl3) δ ppm 8.15 (1H, d, J=2.0 Hz), 7.65 (2H, m), 7.20 (1H, d, J=2.0 Hz), 7.06 (2H, m), 4.11 (5H, m).

1. temperaturethe reaction was cooled to rt
2. extractionAfter extraction with EtOAc
3. extractionthe organic extraction
4. dry with materialwas dried over anhydrous sodium sulfate
5. filtrationAfter filtration and concentration
6. customthe residue was purified on silica gel (0-20% EtOAc in hexanes)