反应详情

温度

130 °C

A mixture of tert-butyl N-(7-chloro-2,6-naphthyridin-3-yl)carbamate (460 mg, 1.65 mmol), (4-methyl-3-pyridyl)boronic acid (450 mg, 3.3 mmol), bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (117 mg, 0.165 mmol) and saturated aqueous sodium carbonate solution (0.5 mL) in acetonitrile (5 mL) was heated under microwave irradiation (Biotage) at 130° C. for 30 minutes. The reaction mixture was diluted with ethyl acetate (150 mL) and washed with water (50 mL). The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo to provide a residue that was purified by flash chromatography (12 g, Silica, 0-10% methanol in dichloromethane). Desired fractions were combined and evaporated in vacuo to afford the title compound as a white solid (190 mg, 34%), which was used in the next step without further purification.

1. washwashed with water (50 mL)
2. customThe organic layer was separated
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto provide a residue that
7. customwas purified by flash chromatography (12 g, Silica, 0-10% methanol in dichloromethane)
8. customevaporated in vacuo