反应详情

[(3-Bromo-4-fluorophenyl)methyl]amine hydrochloride (0.795 g, 3.29 mmol), [3-(hydroxymethyl)phenyl]boronic acid (0.5 g, 3.29 mmol), potassium carbonate (2.275 g, 16.5 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.114 g, 0.1 mmol) were combined in dioxane (10 mL) and water (3 mL). The mixture was microwaved at 150° C. for 30 min. The solvents were evaporated and the residue taken up in EtOAc and H2O. The aqueous phase was extracted 2× with EtOAc. The combined organic phases were dried over anhydrous Na2SO4, filtered and evaporated. The residue was purified by CombiFlash on a silica gel column eluting with 0-100% CH2Cl2/CH2Cl2: 20% MeOH:1% NH4OH to afford the title compound as a viscous oil. LC-MS m/z 231.8 (M+H)+, 1.03 min (ret time).

1. customThe mixture was microwaved at 150° C. for 30 min
2. customThe solvents were evaporated
3. extractionThe aqueous phase was extracted 2× with EtOAc
4. dry with materialThe combined organic phases were dried over anhydrous Na2SO4
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by CombiFlash on a silica gel column
8. washeluting with 0-100% CH2Cl2/CH2Cl2