反应详情

温度

90 °C

Potassium carbonate (5.56 g, 40.3 mmol) and tert-butyl piperazine-1-carboxylate (6.92 g, 37.2 mmol) were combined; methyl 3,4-difluorobenzoate (5.33 g, 31.0 mmol) was added, and the reaction mixture was stirred at 90° C. for 1 d. The mixture was triturated with ethyl acetate (3×5 mL) and the combined organic extracts were filtered, concentrated down to about 5-10 mL, and subjected to flash column chromatography on silica gel (120 g SiO2, hexanes:ethyl acetate 1:0 to 4:1) to afford the title compound as a white solid (4.702 g, 13.90 mmol, 44.9% yield). ESI-MS: m/z 339 (M+H)+.

1. customThe mixture was triturated with ethyl acetate (3×5 mL)
2. filtrationthe combined organic extracts were filtered
3. concentrationconcentrated down to about 5-10 mL