反应详情

温度

120 °C

2,6-Dimethylpiperazine(3.43 g, 30.00 mmol) was added to ethyl 4-fluorobenzoate (1.101 mL, 7.5 mmol), in DMSO (10 mL) warmed to 120° C. under nitrogen. The resulting solution was stirred at 120° C. for 20 h. The reaction mixture was cooled and the solvent was evaporated. The crude product was purified by silica column chromatography, eluting with 10% methanol in dichloromethane containing 1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,5-dimethylpiperazin-1-yl)benzoate (1.490 g, 76%) as a colourless solid.

1. temperatureThe reaction mixture was cooled
2. customthe solvent was evaporated
3. customThe crude product was purified by silica column chromatography
4. washeluting with 10% methanol in dichloromethane containing 1% 0.880 ammonia
5. customPure fractions were evaporated to dryness