反应详情

A mixture of ethyl 3-(2-bromophenylthio)propanoate (7 g, 24 mmol), 5-(2-fluoro-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)pyrazin-2-amine (7.6 g, 24 mmol), Pd(dppf)Cl2.CH2Cl2 (378 mg, 0.52 mmol) and Na2CO3 (5 g, 48 mmol) in dioxane/water (20 mL/5 mL) was stirred at 80° Celsius for 5 hours under N2, then poured into water (60 mL) and extracted with EtOAc (50 mL×3). The combined organic extracts were dried over Na2SO4, filtered, concentrated to dryness and purified by FCC to give ethyl 3-(4′-(5-aminopyrazin-2-yl)-5′-fluorobiphenyl-2-ylthio)propanoate (7.7 g, 80%) as a white solid. MS (ESI): mass calcd. for C21H20FN3O2S, 397.13; m/z found, 397.9 [M+H]+.

1. extractionextracted with EtOAc (50 mL×3)
2. dry with materialThe combined organic extracts were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated to dryness
5. custompurified by FCC