反应详情

温度

85 °C

A 250 ml RB flask was charged with 7′-bromo-4′-fluoro-2′-methoxy-2,6-dihydrospiro[[1,4]oxazine-3,9′-xanthen]-5-amine (2.73 g, 6.94 mmol), bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (0.492 g, 0.694 mmol) and 2-fluoropyridin-3-ylboronic acid (1.467 g, 10.41 mmol). Dioxane (40 mL) and potassium carbonate (1M solution) (20.83 mL, 20.83 mmol) were added and the mixture was flushed with argon and heated at 85° C. for 30 minutes. The mixture was cooled to RT, diluted with EtOAc and the organic layer was separated and concentrated in vacuo to give a yellow semisolid. After trituration with 10 ml of EtOH the solid was filtered, washed with EtOH (2×1 ml) and dried on air overnight to afford 4′-fluoro-7′-(2-fluoropyridin-3-yl)-2′-methoxy-2,6-dihydrospiro[[1,4]oxazine-3,9′-xanthen]-5-amine (2.11 g, 5.15 mmol).

1. customthe mixture was flushed with argon
2. temperatureThe mixture was cooled to RT
3. additiondiluted with EtOAc
4. customthe organic layer was separated
5. concentrationconcentrated in vacuo
6. customto give a yellow semisolid
7. filtrationAfter trituration with 10 ml of EtOH the solid was filtered
8. washwashed with EtOH (2×1 ml)
9. customdried on air overnight