反应详情

温度

95 °C

The product from Step (b) (0.5 g, 1.5 mmol), 4-fluoro phenylboronic acid (0.31 g, 2.2 mmol) and Pd(dppf)2Cl2.CH2Cl2 (0.12 g, 0.15 mmol) were combined in 9 ml of 2:1 Dioxane/2 M K2CO3 The reaction mixture was sealed and heated to 95° C. for 18 h. The resulting biphasic mixture was cooled to room temperature. The phases were separated and the organic phase (top) was filtered. The aqueous layer was extracted once with EtOAc. The combined organic phases were washed with sat'd NaHCO3, water, brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by silica gel chromatography (5% MeOH/CH2Cl2) to afford 0.37 g of the title compound, (100%); MS (ES+) m/e 259 [M+H]+.

1. customwas sealed
2. temperatureThe resulting biphasic mixture was cooled to room temperature
3. customThe phases were separated
4. filtrationthe organic phase (top) was filtered
5. extractionThe aqueous layer was extracted once with EtOAc
6. washThe combined organic phases were washed with sat'd NaHCO3, water, brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated in vacuo
9. customThe residue was purified by silica gel chromatography (5% MeOH/CH2Cl2)