反应详情

温度

100 °C

Ethyl 4-fluorobenzoate (0.753 g, 4.48 mmol) was added to a solution of 1-cyclobutylpiperazine (0.571 g, 4.07 mmol) and potassium carbonate (0.563 g, 4.07 mmol) in DMSO (8 mL) under nitrogen. The resulting solution was stirred at 100° C. for 18 h and evaporated to dryness. The residue was triturated with diethyl ether, filtered, and evaporated and the crude product was purified by silica column chromatography, eluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate (0.387 g, 32.9%) as a white solid.

1. customevaporated to dryness
2. customThe residue was triturated with diethyl ether
3. filtrationfiltered
4. customevaporated
5. customthe crude product was purified by silica column chromatography
6. washeluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM
7. customPure fractions were evaporated to dryness