反应详情

温度

100 °C

A 100 mL round bottom flask was charged with tert-butyl 4-(5-bromo-3-cyanopyrazin-2-yl)piperazine-1-carboxylate (1.0 g, 2.7 mmol), thiophen-2-ylboronic acid (0.52 g, 4.1 mmol), Pd(PPh3)4 (0.31 g, 0.27 mmol), Cs2CO3 (1.4 g, 4.1 mmol), 1,4-dioxane (20 mL) and water (10 mL). The resulting mixture was heated at 100° C. overnight under N2 atmosphere. Work-up: the reaction mixture was poured into brine (80 mL) and extracted with EtOAc (30 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was further purified by flash column chromatography on silica gel with 30% EtOAc in petroleum ether, to afford 700 mg (70%) of the product.

1. extractionextracted with EtOAc (30 mL×3)
2. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
3. concentrationconcentrated in vacuo
4. customThe residue was further purified by flash column chromatography on silica gel with 30% EtOAc in petroleum ether